# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Jonathan Steed' _publ_contact_author_address ; Department of Chemistry University of Durham South Road Durham DH1 3QY UNITED KINGDOM ; _publ_contact_author_email JON.STEED@DURHAM.AC.UK _publ_section_title ; A Modular, Self-Assembled, Separated Ion-Pair Binding System ; loop_ _publ_author_name 'Jonathan Steed' 'Judith A. K. Howard' 'Elinor C. Spencer' 'Derek A. Tocher' 'David R. Turner' data_REV_JWS.CIF _database_code_depnum_ccdc_archive 'CCDC 233238' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common DTAg005 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H30 Ag N7 O6' _chemical_formula_weight 656.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 49.675(4) _cell_length_b 13.4895(10) _cell_length_c 33.477(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.132(7) _cell_angle_gamma 90.00 _cell_volume 18996(3) _cell_formula_units_Z 28 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9408 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7728 _exptl_absorpt_correction_T_max 0.8501 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 57083 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min -61 _diffrn_reflns_limit_h_max 59 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 26.00 _reflns_number_total 18601 _reflns_number_gt 12736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed interface to POVRay' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+64.7025P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18601 _refine_ls_number_parameters 1337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1754 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.075840(11) 0.96588(3) 0.113220(19) 0.04947(16) Uani 1 1 d . . . O1 O 0.16175(8) 0.5905(2) 0.06390(12) 0.0305(7) Uani 1 1 d . . . N1 N 0.11063(9) 0.8868(3) 0.10165(13) 0.0252(8) Uani 1 1 d . . . C1 C 0.20416(12) 0.1259(4) 0.07420(19) 0.0345(11) Uani 1 1 d . . . H1A H 0.2230 0.1451 0.0736 0.052 Uiso 1 1 calc R . . H1B H 0.1890 0.0917 0.0448 0.052 Uiso 1 1 calc R . . H1C H 0.2105 0.0816 0.1010 0.052 Uiso 1 1 calc R . . Ag2 Ag -0.01164(2) 0.54402(6) 0.22236(3) 0.0401(2) Uani 0.50 1 d P . . O2 O -0.02227(7) 0.6249(2) 0.14706(12) 0.0288(7) Uani 1 1 d . . . N2 N 0.12997(8) 0.6320(3) 0.09199(14) 0.0256(8) Uani 1 1 d . . . H2A H 0.1171 0.6064 0.0997 0.031 Uiso 1 1 calc R . . C2 C 0.18873(10) 0.2172(3) 0.07914(16) 0.0255(10) Uani 1 1 d . . . Ag3 Ag 0.21837(3) -0.08720(7) -0.17213(5) 0.0562(3) Uani 0.56 1 d P A 1 O3 O 0.09858(7) 0.1922(3) 0.22332(12) 0.0338(8) Uani 1 1 d . . . N3 N 0.14602(8) 0.4711(3) 0.09591(14) 0.0261(8) Uani 1 1 d . . . H3B H 0.1353 0.4609 0.1097 0.031 Uiso 1 1 calc R . . C3 C 0.20181(11) 0.3104(3) 0.08366(17) 0.0283(10) Uani 1 1 d . . . H3A H 0.2206 0.3163 0.0829 0.034 Uiso 1 1 calc R . . Ag4 Ag 0.155626(10) 0.48330(3) -0.005587(18) 0.03591(16) Uani 0.9167(15) 1 d P B 1 O4 O 0.30726(9) -0.4513(3) -0.21490(16) 0.0603(13) Uani 1 1 d . . . N4 N 0.03350(9) 0.9102(3) 0.11190(14) 0.0254(8) Uani 1 1 d . . . C4 C 0.18849(10) 0.3949(3) 0.08921(17) 0.0274(10) Uani 1 1 d . . . H4A H 0.1983 0.4575 0.0929 0.033 Uiso 1 1 calc R . . O5 O 0.11988(7) -0.4212(2) -0.13932(12) 0.0302(7) Uani 1 1 d . A . N5 N 0.01298(8) 0.6602(3) 0.12482(14) 0.0256(8) Uani 1 1 d . . . H5A H 0.0267 0.6331 0.1191 0.031 Uiso 1 1 calc R . . C5 C 0.16058(10) 0.3884(3) 0.08942(16) 0.0233(9) Uani 1 1 d . . . O6 O 0.23853(7) 0.1262(2) -0.06962(12) 0.0309(8) Uani 1 1 d . . . N6 N -0.00075(8) 0.5005(3) 0.12619(14) 0.0266(9) Uani 1 1 d . . . H6B H 0.0129 0.4890 0.1176 0.032 Uiso 1 1 calc R . . C6 C 0.14702(10) 0.2957(3) 0.08536(16) 0.0255(10) Uani 1 1 d . . . H6A H 0.1282 0.2899 0.0860 0.031 Uiso 1 1 calc R . . O7 O 0.04631(7) 0.1321(2) -0.00671(12) 0.0326(8) Uani 1 1 d . B . N7 N 0.04021(12) 0.4778(4) 0.2504(2) 0.0574(15) Uani 1 1 d . . . C7 C 0.16117(10) 0.2120(3) 0.08045(16) 0.0270(10) Uani 1 1 d . . . H7A H 0.1518 0.1491 0.0779 0.032 Uiso 1 1 calc R . . N8 N 0.05941(8) 0.2270(3) 0.23737(14) 0.0288(9) Uani 1 1 d . . . H8A H 0.0452 0.2002 0.2421 0.035 Uiso 1 1 calc R . . C8 C 0.14714(10) 0.5666(3) 0.08247(16) 0.0261(10) Uani 1 1 d . . . N9 N 0.07003(9) 0.0660(3) 0.22918(14) 0.0286(9) Uani 1 1 d . . . H9A H 0.0537 0.0541 0.2319 0.034 Uiso 1 1 calc R . . C9 C 0.13118(10) 0.7357(3) 0.09042(16) 0.0229(9) Uani 1 1 d . . . N10 N 0.25245(10) -0.1571(4) -0.18429(15) 0.0403(11) Uani 1 1 d . . . C10 C 0.15106(11) 0.7889(4) 0.08083(17) 0.0294(11) Uani 1 1 d . . . H10A H 0.1650 0.7559 0.0739 0.035 Uiso 1 1 calc R . . N11 N 0.27438(9) -0.4128(3) -0.18848(15) 0.0366(10) Uani 1 1 d . A . H11B H 0.2617 -0.4386 -0.1804 0.044 Uiso 1 1 calc R . . C11 C 0.15000(11) 0.8919(3) 0.08163(17) 0.0306(11) Uani 1 1 d . . . H11A H 0.1632 0.9301 0.0749 0.037 Uiso 1 1 calc R . . N12 N 0.28799(9) -0.5737(3) -0.19038(15) 0.0366(10) Uani 1 1 d . . . H12B H 0.2760 -0.5854 -0.1789 0.044 Uiso 1 1 calc R . . C12 C 0.12969(11) 0.9392(3) 0.09229(16) 0.0275(10) Uani 1 1 d . . . H12A H 0.1293 1.0095 0.0930 0.033 Uiso 1 1 calc R . . N13 N 0.17412(10) -0.1378(3) -0.17885(16) 0.0362(10) Uani 1 1 d . . . C13 C 0.11129(10) 0.7888(3) 0.10044(15) 0.0240(9) Uani 1 1 d . . . H13A H 0.0975 0.7526 0.1067 0.029 Uiso 1 1 calc R . . N14 N 0.15583(8) -0.3877(3) -0.16056(14) 0.0262(8) Uani 1 1 d . A . H14B H 0.1700 -0.4148 -0.1653 0.031 Uiso 1 1 calc R . . C14 C 0.01449(10) 0.9656(3) 0.12000(16) 0.0249(9) Uani 1 1 d . . . H14A H 0.0157 1.0358 0.1192 0.030 Uiso 1 1 calc R . . N15 N 0.14306(8) -0.5471(3) -0.15646(13) 0.0243(8) Uani 1 1 d . A . H15B H 0.1573 -0.5591 -0.1638 0.029 Uiso 1 1 calc R . . C15 C -0.00675(11) 0.9229(3) 0.12948(17) 0.0287(10) Uani 1 1 d . . . H15A H -0.0203 0.9638 0.1345 0.034 Uiso 1 1 calc R . . N16 N 0.18651(9) 0.4102(3) -0.02784(14) 0.0278(9) Uani 1 1 d . . . C16 C -0.00845(10) 0.8213(3) 0.13174(16) 0.0255(10) Uani 1 1 d . . . H16A H -0.0230 0.7914 0.1384 0.031 Uiso 1 1 calc R . . N17 N 0.20203(8) 0.1595(3) -0.04960(13) 0.0233(8) Uani 1 1 d . B . H17A H 0.1882 0.1323 -0.0442 0.028 Uiso 1 1 calc R . . C17 C 0.01156(10) 0.7637(3) 0.12405(16) 0.0218(9) Uani 1 1 d . . . N18 N 0.21340(8) -0.0008(3) -0.05723(13) 0.0226(8) Uani 1 1 d . . . H18B H 0.1978 -0.0135 -0.0528 0.027 Uiso 1 1 calc R . . C18 C 0.03194(10) 0.8124(3) 0.11374(15) 0.0223(9) Uani 1 1 d . . . H18A H 0.0454 0.7735 0.1077 0.027 Uiso 1 1 calc R . . N19 N 0.10750(9) 0.4213(3) -0.02597(15) 0.0330(9) Uani 1 1 d . . . C19 C -0.00493(10) 0.5964(3) 0.13358(16) 0.0233(9) Uani 1 1 d . . . O20 O 0.07697(10) 1.1308(3) 0.08981(15) 0.0496(10) Uani 1 1 d . . . N20 N 0.08249(8) 0.1682(3) -0.02716(13) 0.0266(9) Uani 1 1 d . B . H20A H 0.0952 0.1422 -0.0352 0.032 Uiso 1 1 calc R . . C20 C -0.01607(10) 0.4165(3) 0.13086(16) 0.0248(10) Uani 1 1 d . . . O21 O 0.00922(18) 0.7005(5) 0.2393(3) 0.0419(18) Uani 0.50 1 d P . . N21 N 0.07115(9) 0.0067(3) -0.02122(14) 0.0280(9) Uani 1 1 d . B . H21B H 0.0856 -0.0053 -0.0281 0.034 Uiso 1 1 calc R . . C21 C -0.00413(10) 0.3243(3) 0.13078(16) 0.0252(10) Uani 1 1 d . . . H21A H 0.0139 0.3194 0.1281 0.030 Uiso 1 1 calc R . . O22 O 0.22084(19) 0.0764(6) -0.1925(4) 0.063(2) Uani 0.56 1 d P A 1 C22 C -0.01804(10) 0.2387(3) 0.13461(17) 0.0267(10) Uani 1 1 d . . . H22A H -0.0093 0.1760 0.1348 0.032 Uiso 1 1 calc R . . O23 O 0.15261(10) 0.6373(3) -0.04644(14) 0.0398(9) Uani 0.9167(15) 1 d P B 1 C23 C -0.04459(10) 0.2430(3) 0.13826(16) 0.0248(10) Uani 1 1 d . . . O24 O 0.0000 0.1745(4) 0.2500 0.071(2) Uani 1 2 d S . . C24 C -0.05656(12) 0.3359(3) 0.1379(2) 0.0386(13) Uani 1 1 d . . . H24A H -0.0748 0.3408 0.1401 0.046 Uiso 1 1 calc R . . O25 O 0.01758(9) 0.0363(3) 0.24103(16) 0.0537(11) Uani 1 1 d . . . C25 C -0.04268(12) 0.4221(4) 0.1344(2) 0.0422(14) Uani 1 1 d . . . H25A H -0.0514 0.4848 0.1344 0.051 Uiso 1 1 calc R . . C26 C -0.06033(12) 0.1502(3) 0.14113(18) 0.0321(11) Uani 1 1 d . . . H26A H -0.0789 0.1681 0.1426 0.048 Uiso 1 1 calc R . . H26B H -0.0452 0.1129 0.1695 0.048 Uiso 1 1 calc R . . H26C H -0.0671 0.1092 0.1132 0.048 Uiso 1 1 calc R . . C27 C 0.13033(12) -0.2864(4) 0.21795(18) 0.0349(11) Uani 1 1 d . . . H27A H 0.1468 -0.2696 0.2114 0.052 Uiso 1 1 calc R . . H27B H 0.1145 -0.3298 0.1930 0.052 Uiso 1 1 calc R . . H27C H 0.1400 -0.3205 0.2484 0.052 Uiso 1 1 calc R . . C28 C 0.11437(10) -0.1929(3) 0.21956(16) 0.0265(10) Uani 1 1 d . . . C29 C 0.12420(10) -0.0996(3) 0.21406(17) 0.0286(10) Uani 1 1 d . . . H29A H 0.1409 -0.0953 0.2083 0.034 Uiso 1 1 calc R . . C30 C 0.11018(10) -0.0128(3) 0.21685(17) 0.0284(10) Uani 1 1 d . . . H30A H 0.1174 0.0496 0.2131 0.034 Uiso 1 1 calc R . . C31 C 0.08544(10) -0.0175(3) 0.22521(16) 0.0263(10) Uani 1 1 d . . . C32 C 0.07548(11) -0.1099(4) 0.23054(16) 0.0298(11) Uani 1 1 d . . . H32A H 0.0588 -0.1144 0.2365 0.036 Uiso 1 1 calc R . . C33 C 0.08951(11) -0.1950(4) 0.22736(16) 0.0301(11) Uani 1 1 d . . . H33A H 0.0820 -0.2574 0.2306 0.036 Uiso 1 1 calc R . . C34 C 0.07760(10) 0.1631(3) 0.22926(16) 0.0249(10) Uani 1 1 d . . . C35 C 0.06130(10) 0.3300(3) 0.23879(16) 0.0257(10) Uani 1 1 d . . . C36 C 0.08141(12) 0.3866(4) 0.23090(19) 0.0362(12) Uani 1 1 d . . . H36A H 0.0959 0.3557 0.2246 0.043 Uiso 1 1 calc R . . C37 C 0.07992(11) 0.4888(4) 0.23236(18) 0.0359(12) Uani 1 1 d . . . H37A H 0.0931 0.5287 0.2264 0.043 Uiso 1 1 calc R . . C38 C 0.05929(12) 0.5322(4) 0.24252(19) 0.0384(12) Uani 1 1 d . . . H38A H 0.0586 0.6025 0.2440 0.046 Uiso 1 1 calc R . . C39 C 0.04142(12) 0.3802(4) 0.2486(2) 0.0420(13) Uani 1 1 d . . . H39A H 0.0277 0.3424 0.2544 0.050 Uiso 1 1 calc R . . C40 C 0.34328(14) -0.9200(4) -0.2167(2) 0.0483(14) Uani 1 1 d . . . H40A H 0.3317 -0.9786 -0.2164 0.072 Uiso 1 1 calc R . . H40B H 0.3656 -0.9245 -0.1908 0.072 Uiso 1 1 calc R . . H40C H 0.3421 -0.9166 -0.2468 0.072 Uiso 1 1 calc R . . C41 C 0.32863(12) -0.8286(4) -0.21060(18) 0.0376(12) Uani 1 1 d . . . C42 C 0.34131(13) -0.7361(4) -0.2080(2) 0.0449(14) Uani 1 1 d . . . H42A H 0.3594 -0.7309 -0.2107 0.054 Uiso 1 1 calc R . . C43 C 0.32861(12) -0.6503(4) -0.20160(19) 0.0403(13) Uani 1 1 d . . . H43A H 0.3380 -0.5877 -0.1996 0.048 Uiso 1 1 calc R . . C44 C 0.30188(11) -0.6572(4) -0.19808(17) 0.0315(11) Uani 1 1 d . . . C45 C 0.28877(11) -0.7487(4) -0.20091(17) 0.0355(12) Uani 1 1 d . . . H45A H 0.2705 -0.7540 -0.1987 0.043 Uiso 1 1 calc R . . C46 C 0.30215(12) -0.8337(4) -0.20695(17) 0.0382(12) Uani 1 1 d . . . H46A H 0.2929 -0.8965 -0.2086 0.046 Uiso 1 1 calc R . . C47 C 0.29118(11) -0.4781(4) -0.19873(18) 0.0387(13) Uani 1 1 d . . . C48 C 0.27558(10) -0.3084(4) -0.18973(17) 0.0333(12) Uani 1 1 d . . . C49 C 0.29697(12) -0.2554(5) -0.1961(2) 0.0471(15) Uani 1 1 d . A . H49A H 0.3124 -0.2885 -0.1997 0.057 Uiso 1 1 calc R . . C50 C 0.29516(12) -0.1522(5) -0.1971(2) 0.0493(15) Uani 1 1 d . . . H50A H 0.3092 -0.1139 -0.2020 0.059 Uiso 1 1 calc R A . C51 C 0.27284(12) -0.1059(5) -0.19083(19) 0.0432(14) Uani 1 1 d . A . H51A H 0.2720 -0.0355 -0.1912 0.052 Uiso 1 1 calc R . . C52 C 0.25393(11) -0.2558(4) -0.18392(17) 0.0352(12) Uani 1 1 d . A . H52A H 0.2394 -0.2921 -0.1794 0.042 Uiso 1 1 calc R . . C53 C 0.17289(11) -0.2357(4) -0.17551(18) 0.0335(12) Uani 1 1 d . A . H53A H 0.1861 -0.2751 -0.1818 0.040 Uiso 1 1 calc R . . C54 C 0.15351(10) -0.2840(3) -0.16335(16) 0.0229(9) Uani 1 1 d . . . C55 C 0.13370(10) -0.2258(3) -0.15528(16) 0.0276(10) Uani 1 1 d . A . H55A H 0.1197 -0.2552 -0.1475 0.033 Uiso 1 1 calc R . . C56 C 0.13503(11) -0.1239(3) -0.15895(17) 0.0302(11) Uani 1 1 d . . . H56A H 0.1217 -0.0825 -0.1538 0.036 Uiso 1 1 calc R A . C57 C 0.15556(11) -0.0820(4) -0.17009(17) 0.0320(11) Uani 1 1 d . A . H57A H 0.1566 -0.0119 -0.1716 0.038 Uiso 1 1 calc R . . C58 C 0.13822(10) -0.4514(3) -0.15120(16) 0.0231(9) Uani 1 1 d . . . C59 C 0.12785(10) -0.6312(3) -0.15156(15) 0.0215(9) Uani 1 1 d . . . C60 C 0.13877(10) -0.7233(3) -0.15521(16) 0.0256(10) Uani 1 1 d . A . H60A H 0.1562 -0.7277 -0.1593 0.031 Uiso 1 1 calc R . . C61 C 0.12423(11) -0.8092(3) -0.15284(17) 0.0296(10) Uani 1 1 d . . . H61A H 0.1319 -0.8719 -0.1555 0.035 Uiso 1 1 calc R A . C62 C 0.09858(11) -0.8052(3) -0.14667(16) 0.0275(10) Uani 1 1 d . A . C63 C 0.08848(11) -0.7134(4) -0.14242(18) 0.0323(11) Uani 1 1 d . . . H63A H 0.0713 -0.7092 -0.1377 0.039 Uiso 1 1 calc R A . C64 C 0.10253(11) -0.6263(3) -0.14486(18) 0.0312(11) Uani 1 1 d . A . H64A H 0.0949 -0.5639 -0.1420 0.037 Uiso 1 1 calc R . . C65 C 0.08222(12) -0.8989(4) -0.14582(19) 0.0361(12) Uani 1 1 d . . . H65A H 0.0644 -0.8817 -0.1424 0.054 Uiso 1 1 calc R A . H65B H 0.0974 -0.9403 -0.1192 0.054 Uiso 1 1 calc R . . H65C H 0.0743 -0.9355 -0.1753 0.054 Uiso 1 1 calc R . . C66 C 0.27521(11) -0.3514(3) -0.06616(18) 0.0317(11) Uani 1 1 d . . . H66A H 0.2641 -0.4094 -0.0641 0.048 Uiso 1 1 calc R . . H66B H 0.2972 -0.3511 -0.0393 0.048 Uiso 1 1 calc R . . H66C H 0.2750 -0.3542 -0.0956 0.048 Uiso 1 1 calc R . . C67 C 0.25880(10) -0.2589(3) -0.06542(16) 0.0241(9) Uani 1 1 d . . . C68 C 0.26919(10) -0.1654(3) -0.06861(16) 0.0249(10) Uani 1 1 d . . . H68A H 0.2869 -0.1605 -0.0722 0.030 Uiso 1 1 calc R . . C69 C 0.25482(10) -0.0786(3) -0.06679(16) 0.0236(10) Uani 1 1 d . . . H69A H 0.2625 -0.0160 -0.0695 0.028 Uiso 1 1 calc R . . C70 C 0.22907(9) -0.0840(3) -0.06105(15) 0.0204(9) Uani 1 1 d . . . C71 C 0.21799(10) -0.1771(3) -0.05833(16) 0.0256(10) Uani 1 1 d . . . H71A H 0.2003 -0.1822 -0.0548 0.031 Uiso 1 1 calc R . . C72 C 0.23260(10) -0.2619(3) -0.06073(17) 0.0281(10) Uani 1 1 d . . . H72A H 0.2245 -0.3246 -0.0591 0.034 Uiso 1 1 calc R . . C73 C 0.21942(10) 0.0960(3) -0.05952(15) 0.0216(9) Uani 1 1 d . . . C74 C 0.20414(9) 0.2627(3) -0.04728(15) 0.0206(9) Uani 1 1 d . . . C75 C 0.22195(11) 0.3207(3) -0.05976(17) 0.0275(10) Uani 1 1 d . B . H75A H 0.2343 0.2907 -0.0704 0.033 Uiso 1 1 calc R . . C76 C 0.22107(11) 0.4225(3) -0.05617(16) 0.0286(10) Uani 1 1 d . . . H76A H 0.2329 0.4633 -0.0646 0.034 Uiso 1 1 calc R B . C77 C 0.20329(10) 0.4650(3) -0.04048(16) 0.0261(10) Uani 1 1 d . B . H77A H 0.2028 0.5352 -0.0385 0.031 Uiso 1 1 calc R . . C78 C 0.18695(10) 0.3121(3) -0.03133(16) 0.0259(10) Uani 1 1 d . B . H78A H 0.1749 0.2736 -0.0225 0.031 Uiso 1 1 calc R . . C79 C 0.10459(11) 0.3230(3) -0.02870(17) 0.0289(10) Uani 1 1 d . B . H79A H 0.1190 0.2860 -0.0332 0.035 Uiso 1 1 calc R . . C80 C 0.08167(10) 0.2713(4) -0.02533(16) 0.0261(10) Uani 1 1 d . . . C81 C 0.05996(11) 0.3272(4) -0.02020(18) 0.0343(12) Uani 1 1 d . B . H81A H 0.0435 0.2958 -0.0184 0.041 Uiso 1 1 calc R . . C82 C 0.06289(12) 0.4281(4) -0.01789(19) 0.0387(12) Uani 1 1 d . . . H82A H 0.0486 0.4673 -0.0139 0.046 Uiso 1 1 calc R B . C83 C 0.08662(11) 0.4739(4) -0.02129(19) 0.0381(12) Uani 1 1 d . B . H83A H 0.0880 0.5442 -0.0203 0.046 Uiso 1 1 calc R . . C84 C 0.06526(10) 0.1033(4) -0.01763(16) 0.0250(10) Uani 1 1 d . . . C85 C 0.05648(10) -0.0770(3) -0.01506(16) 0.0239(9) Uani 1 1 d . . . C86 C 0.06758(11) -0.1693(4) -0.01831(17) 0.0298(11) Uani 1 1 d . B . H86A H 0.0844 -0.1734 -0.0239 0.036 Uiso 1 1 calc R . . C87 C 0.05449(11) -0.2548(4) -0.01348(17) 0.0315(11) Uani 1 1 d . . . H87A H 0.0623 -0.3171 -0.0162 0.038 Uiso 1 1 calc R B . C88 C 0.02997(10) -0.2524(4) -0.00475(16) 0.0282(10) Uani 1 1 d . B . C89 C 0.01932(10) -0.1597(4) -0.00164(17) 0.0289(10) Uani 1 1 d . . . H89A H 0.0026 -0.1555 0.0042 0.035 Uiso 1 1 calc R B . C90 C 0.03206(11) -0.0728(4) -0.00677(18) 0.0313(11) Uani 1 1 d . B . H90A H 0.0240 -0.0105 -0.0046 0.038 Uiso 1 1 calc R . . C91 C 0.01506(12) -0.3464(4) -0.00076(19) 0.0377(12) Uani 1 1 d . . . H91A H -0.0015 -0.3296 0.0057 0.057 Uiso 1 1 calc R B . H91B H 0.0314 -0.3871 0.0251 0.057 Uiso 1 1 calc R . . H91C H 0.0056 -0.3835 -0.0304 0.057 Uiso 1 1 calc R . . O100 O 0.04823(8) 0.4568(3) 0.10496(14) 0.0426(9) Uani 1 1 d . . . N100 N 0.06874(8) 0.5152(3) 0.10875(13) 0.0255(8) Uani 1 1 d . . . O101 O 0.08986(9) 0.4854(3) 0.10297(16) 0.0525(11) Uani 1 1 d . . . N101 N 0.14194(8) 0.0235(3) -0.03548(14) 0.0254(8) Uani 1 1 d . . . O102 O 0.06746(8) 0.6044(2) 0.11811(14) 0.0418(9) Uani 1 1 d . . . N102 N 0.21069(9) -0.5322(3) -0.17836(14) 0.0295(9) Uani 1 1 d . . . O103 O 0.13862(9) 0.1142(3) -0.03237(14) 0.0497(10) Uani 1 1 d . . . N103 N 0.0000 0.0833(4) 0.2500 0.0313(13) Uani 1 2 d S . . O104 O 0.16283(9) -0.0097(3) -0.04055(17) 0.0550(11) Uani 1 1 d . . . O105 O 0.12344(8) -0.0343(3) -0.03287(15) 0.0446(10) Uani 1 1 d . . . O106 O 0.22995(8) -0.5623(3) -0.18846(15) 0.0460(10) Uani 1 1 d . . . O107 O 0.21129(9) -0.4452(3) -0.16594(14) 0.0458(9) Uani 1 1 d . . . O108 O 0.19024(8) -0.5900(3) -0.18108(14) 0.0405(9) Uani 1 1 d . . . Ag3A Ag 0.20547(3) -0.07134(8) -0.20289(5) 0.0468(3) Uani 0.44 1 d P A 2 Ag4A Ag 0.13660(14) 0.4818(3) -0.0557(2) 0.049(2) Uani 0.0833(15) 1 d P B 2 O22A O 0.2232(2) 0.0823(5) -0.1611(3) 0.0322(19) Uani 0.44 1 d P A 2 O23A O 0.1377(12) 0.633(4) -0.0366(18) 0.052(13) Uiso 0.0833(15) 1 d P B 2 C20M C 0.06860(15) 1.2171(4) 0.1047(2) 0.0480(14) Uani 1 1 d . . . H20B H 0.0809 1.2200 0.1393 0.072 Uiso 1 1 calc R . . H20C H 0.0459 1.2153 0.0931 0.072 Uiso 1 1 calc R . . H20D H 0.0732 1.2758 0.0922 0.072 Uiso 1 1 calc R . . C21M C 0.0000 0.7899(6) 0.2500 0.052(2) Uani 1 2 d S . . C22M C 0.21017(15) 0.1709(4) -0.1835(2) 0.0491(15) Uani 1 1 d . . . C23M C 0.14314(13) 0.7296(4) -0.03735(19) 0.0383(12) Uani 1 1 d . . . H23A H 0.1216 0.7238 -0.0436 0.057 Uiso 1 1 calc R B 1 H23B H 0.1435 0.7806 -0.0579 0.057 Uiso 1 1 calc R B 1 H23C H 0.1578 0.7482 -0.0043 0.057 Uiso 1 1 calc R B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0586(3) 0.0235(2) 0.1036(4) 0.0036(2) 0.0683(3) -0.00004(18) O1 0.0347(18) 0.0274(17) 0.048(2) 0.0048(15) 0.0346(17) 0.0011(14) N1 0.0247(19) 0.029(2) 0.029(2) -0.0012(16) 0.0185(18) -0.0024(15) C1 0.036(3) 0.031(3) 0.046(3) 0.002(2) 0.028(3) 0.004(2) Ag2 0.0519(5) 0.0261(4) 0.0716(5) -0.0007(4) 0.0527(5) -0.0029(3) O2 0.0314(17) 0.0255(16) 0.046(2) -0.0027(14) 0.0316(17) -0.0015(13) N2 0.0241(19) 0.0247(19) 0.043(2) 0.0021(17) 0.0281(19) -0.0017(15) C2 0.024(2) 0.032(2) 0.024(2) 0.0005(19) 0.015(2) 0.0006(19) Ag3 0.0660(7) 0.0322(4) 0.1059(9) 0.0038(6) 0.0696(7) -0.0074(4) O3 0.0283(18) 0.0393(19) 0.047(2) 0.0069(16) 0.0290(17) 0.0037(15) N3 0.0228(19) 0.031(2) 0.039(2) 0.0032(17) 0.0267(18) -0.0014(16) C3 0.024(2) 0.033(3) 0.040(3) 0.001(2) 0.025(2) -0.0027(19) Ag4 0.0454(3) 0.0217(2) 0.0648(4) -0.00078(19) 0.0456(3) 0.00177(17) O4 0.051(2) 0.071(3) 0.092(3) 0.048(3) 0.060(3) 0.024(2) N4 0.025(2) 0.0230(19) 0.037(2) -0.0028(16) 0.0228(18) -0.0009(15) C4 0.025(2) 0.027(2) 0.041(3) 0.003(2) 0.025(2) -0.0017(18) O5 0.0313(17) 0.0300(17) 0.043(2) -0.0090(15) 0.0291(16) -0.0038(14) N5 0.0231(19) 0.0224(19) 0.042(2) -0.0003(17) 0.0248(19) 0.0013(15) C5 0.017(2) 0.034(2) 0.027(2) 0.0029(19) 0.017(2) 0.0015(18) O6 0.0326(18) 0.0273(17) 0.053(2) 0.0073(15) 0.0365(18) 0.0034(13) N6 0.0197(18) 0.0227(19) 0.048(3) 0.0039(17) 0.0254(18) 0.0011(14) C6 0.015(2) 0.039(3) 0.028(3) 0.003(2) 0.015(2) -0.0047(18) O7 0.0281(17) 0.0378(19) 0.047(2) -0.0084(16) 0.0297(17) -0.0025(14) N7 0.058(3) 0.040(3) 0.112(5) -0.027(3) 0.071(3) -0.017(2) C7 0.024(2) 0.028(2) 0.030(3) 0.0037(19) 0.016(2) -0.0048(19) N8 0.0185(19) 0.037(2) 0.042(2) 0.0054(18) 0.0228(18) 0.0016(16) C8 0.020(2) 0.032(2) 0.034(3) 0.004(2) 0.019(2) 0.0031(18) N9 0.0223(19) 0.035(2) 0.042(2) 0.0000(18) 0.0257(19) -0.0037(16) C9 0.016(2) 0.028(2) 0.030(3) -0.0015(19) 0.016(2) -0.0045(17) N10 0.039(2) 0.053(3) 0.040(3) -0.010(2) 0.028(2) -0.019(2) C10 0.024(2) 0.033(3) 0.042(3) 0.000(2) 0.025(2) -0.0033(19) N11 0.020(2) 0.053(3) 0.044(3) 0.014(2) 0.022(2) -0.0003(18) C11 0.027(2) 0.032(3) 0.043(3) 0.003(2) 0.026(2) -0.0033(19) N12 0.027(2) 0.055(3) 0.042(3) 0.006(2) 0.027(2) -0.0073(19) C12 0.029(2) 0.025(2) 0.035(3) 0.003(2) 0.022(2) -0.0018(19) N13 0.038(2) 0.026(2) 0.057(3) -0.0128(19) 0.034(2) -0.0112(18) C13 0.020(2) 0.033(2) 0.026(3) 0.0027(19) 0.017(2) -0.0004(18) N14 0.0230(19) 0.0268(19) 0.040(2) -0.0055(17) 0.0243(18) -0.0028(15) C14 0.024(2) 0.019(2) 0.035(3) 0.0006(18) 0.018(2) 0.0011(17) N15 0.0218(19) 0.0272(19) 0.034(2) 0.0021(16) 0.0219(18) 0.0007(15) C15 0.025(2) 0.030(2) 0.039(3) -0.005(2) 0.022(2) 0.0021(19) N16 0.026(2) 0.0236(19) 0.045(2) 0.0030(17) 0.0262(19) 0.0032(15) C16 0.019(2) 0.030(2) 0.034(3) -0.001(2) 0.019(2) -0.0012(18) N17 0.0197(18) 0.0228(18) 0.038(2) -0.0031(16) 0.0222(18) -0.0027(14) C17 0.017(2) 0.022(2) 0.029(2) -0.0008(18) 0.0141(19) -0.0001(17) N18 0.0179(17) 0.0244(19) 0.037(2) -0.0040(16) 0.0225(17) -0.0029(14) C18 0.022(2) 0.024(2) 0.028(2) -0.0045(18) 0.018(2) -0.0003(17) N19 0.023(2) 0.030(2) 0.049(3) 0.0007(19) 0.021(2) 0.0046(16) C19 0.020(2) 0.021(2) 0.032(3) 0.0037(18) 0.016(2) 0.0001(17) O20 0.069(3) 0.0244(18) 0.069(3) 0.0039(18) 0.046(2) 0.0039(18) N20 0.0183(18) 0.031(2) 0.040(2) -0.0044(17) 0.0218(18) 0.0007(15) C20 0.021(2) 0.020(2) 0.037(3) 0.0024(19) 0.018(2) 0.0023(17) O21 0.050(5) 0.029(4) 0.052(5) 0.000(3) 0.031(4) 0.006(3) N21 0.0216(19) 0.035(2) 0.039(2) 0.0022(17) 0.0242(18) 0.0034(16) C21 0.019(2) 0.029(2) 0.034(3) -0.0062(19) 0.018(2) -0.0025(18) O22 0.058(5) 0.038(4) 0.094(7) 0.005(4) 0.041(5) 0.010(4) C22 0.022(2) 0.022(2) 0.038(3) 0.0000(19) 0.017(2) 0.0042(18) O23 0.050(2) 0.0265(19) 0.048(2) 0.0059(17) 0.030(2) 0.0143(17) C23 0.023(2) 0.024(2) 0.030(3) -0.0010(19) 0.016(2) -0.0031(18) O24 0.092(5) 0.024(3) 0.045(4) 0.000 0.001(3) 0.000 C24 0.033(3) 0.023(2) 0.078(4) 0.005(2) 0.042(3) 0.002(2) O25 0.041(2) 0.068(3) 0.081(3) -0.014(2) 0.052(2) -0.009(2) C25 0.035(3) 0.021(2) 0.093(5) 0.007(3) 0.049(3) 0.005(2) C26 0.034(3) 0.023(2) 0.046(3) 0.000(2) 0.026(2) -0.004(2) C27 0.030(3) 0.037(3) 0.040(3) 0.001(2) 0.021(2) -0.001(2) C28 0.020(2) 0.033(2) 0.025(3) 0.0019(19) 0.011(2) -0.0003(19) C29 0.022(2) 0.036(3) 0.037(3) -0.002(2) 0.022(2) -0.0037(19) C30 0.021(2) 0.032(2) 0.041(3) -0.007(2) 0.022(2) -0.0064(19) C31 0.020(2) 0.034(2) 0.029(3) 0.000(2) 0.016(2) -0.0007(19) C32 0.022(2) 0.044(3) 0.030(3) 0.005(2) 0.019(2) -0.001(2) C33 0.028(2) 0.034(3) 0.030(3) 0.003(2) 0.016(2) -0.004(2) C34 0.017(2) 0.036(3) 0.026(3) 0.0032(19) 0.013(2) 0.0034(18) C35 0.017(2) 0.035(3) 0.026(3) 0.0023(19) 0.012(2) -0.0015(18) C36 0.030(3) 0.044(3) 0.051(3) 0.010(2) 0.032(3) 0.004(2) C37 0.027(3) 0.040(3) 0.045(3) 0.005(2) 0.023(2) -0.003(2) C38 0.034(3) 0.039(3) 0.053(3) -0.006(2) 0.030(3) -0.005(2) C39 0.038(3) 0.038(3) 0.070(4) -0.013(3) 0.043(3) -0.010(2) C40 0.058(4) 0.052(4) 0.049(4) -0.003(3) 0.039(3) -0.010(3) C41 0.038(3) 0.046(3) 0.032(3) -0.007(2) 0.021(2) -0.013(2) C42 0.047(3) 0.053(3) 0.058(4) -0.005(3) 0.044(3) -0.014(3) C43 0.033(3) 0.052(3) 0.053(3) -0.009(3) 0.035(3) -0.016(2) C44 0.026(2) 0.048(3) 0.027(3) 0.001(2) 0.019(2) -0.006(2) C45 0.019(2) 0.064(4) 0.028(3) 0.005(2) 0.016(2) -0.014(2) C46 0.035(3) 0.052(3) 0.028(3) 0.003(2) 0.017(2) -0.014(2) C47 0.017(2) 0.066(4) 0.034(3) 0.022(3) 0.014(2) 0.005(2) C48 0.016(2) 0.054(3) 0.027(3) 0.013(2) 0.009(2) -0.005(2) C49 0.021(3) 0.068(4) 0.056(4) 0.025(3) 0.023(3) 0.003(2) C50 0.028(3) 0.066(4) 0.053(4) 0.016(3) 0.021(3) -0.013(3) C51 0.034(3) 0.055(3) 0.039(3) 0.003(3) 0.018(3) -0.017(3) C52 0.025(3) 0.051(3) 0.036(3) -0.004(2) 0.020(2) -0.014(2) C53 0.033(3) 0.030(3) 0.052(3) -0.014(2) 0.033(3) -0.012(2) C54 0.017(2) 0.026(2) 0.026(2) -0.0088(18) 0.0122(19) -0.0039(17) C55 0.022(2) 0.033(2) 0.033(3) -0.001(2) 0.018(2) 0.0015(19) C56 0.030(3) 0.030(2) 0.034(3) 0.000(2) 0.019(2) 0.009(2) C57 0.032(3) 0.027(2) 0.041(3) -0.006(2) 0.022(2) -0.002(2) C58 0.016(2) 0.029(2) 0.026(2) -0.0036(18) 0.0120(19) -0.0021(17) C59 0.018(2) 0.026(2) 0.023(2) 0.0028(18) 0.0120(19) 0.0008(17) C60 0.019(2) 0.031(2) 0.032(3) -0.0027(19) 0.017(2) 0.0014(18) C61 0.029(2) 0.027(2) 0.036(3) -0.002(2) 0.019(2) 0.0005(19) C62 0.026(2) 0.030(2) 0.029(3) 0.0041(19) 0.017(2) -0.0018(19) C63 0.027(2) 0.035(3) 0.046(3) 0.004(2) 0.027(2) 0.005(2) C64 0.030(3) 0.026(2) 0.051(3) 0.001(2) 0.031(2) 0.0030(19) C65 0.037(3) 0.030(3) 0.048(3) -0.002(2) 0.027(3) -0.002(2) C66 0.027(2) 0.025(2) 0.048(3) 0.001(2) 0.023(2) 0.0025(19) C67 0.019(2) 0.024(2) 0.029(3) -0.0009(18) 0.013(2) 0.0024(17) C68 0.020(2) 0.027(2) 0.035(3) -0.0016(19) 0.019(2) -0.0019(18) C69 0.021(2) 0.020(2) 0.039(3) -0.0076(19) 0.022(2) -0.0086(17) C70 0.014(2) 0.028(2) 0.025(2) -0.0026(18) 0.0136(18) -0.0015(17) C71 0.020(2) 0.029(2) 0.036(3) 0.003(2) 0.020(2) -0.0018(18) C72 0.025(2) 0.022(2) 0.041(3) 0.007(2) 0.020(2) -0.0003(18) C73 0.016(2) 0.027(2) 0.022(2) 0.0005(18) 0.0110(19) -0.0010(17) C74 0.014(2) 0.024(2) 0.024(2) -0.0012(17) 0.0096(18) -0.0003(16) C75 0.026(2) 0.028(2) 0.039(3) -0.005(2) 0.025(2) -0.0020(19) C76 0.026(2) 0.033(3) 0.034(3) 0.002(2) 0.021(2) -0.0041(19) C77 0.024(2) 0.022(2) 0.035(3) -0.0026(19) 0.018(2) -0.0025(18) C78 0.025(2) 0.026(2) 0.037(3) -0.0002(19) 0.023(2) -0.0002(18) C79 0.023(2) 0.028(2) 0.040(3) 0.001(2) 0.020(2) 0.0059(18) C80 0.017(2) 0.037(3) 0.026(3) -0.005(2) 0.012(2) 0.0018(18) C81 0.020(2) 0.042(3) 0.045(3) -0.006(2) 0.021(2) 0.002(2) C82 0.029(3) 0.040(3) 0.052(3) -0.007(2) 0.025(3) 0.008(2) C83 0.030(3) 0.035(3) 0.053(3) -0.001(2) 0.024(3) 0.008(2) C84 0.016(2) 0.038(3) 0.026(3) -0.004(2) 0.015(2) 0.0008(18) C85 0.018(2) 0.030(2) 0.028(3) -0.0002(19) 0.015(2) 0.0019(18) C86 0.023(2) 0.038(3) 0.035(3) -0.005(2) 0.020(2) 0.004(2) C87 0.029(3) 0.029(2) 0.038(3) -0.005(2) 0.019(2) 0.007(2) C88 0.020(2) 0.035(3) 0.029(3) -0.004(2) 0.013(2) -0.0011(19) C89 0.020(2) 0.039(3) 0.035(3) 0.000(2) 0.020(2) 0.0019(19) C90 0.025(2) 0.033(3) 0.046(3) 0.003(2) 0.025(2) 0.006(2) C91 0.037(3) 0.035(3) 0.049(3) -0.005(2) 0.028(3) 0.001(2) O100 0.037(2) 0.037(2) 0.077(3) -0.0156(18) 0.045(2) -0.0160(16) N100 0.0210(19) 0.0261(19) 0.035(2) 0.0021(16) 0.0182(18) 0.0008(15) O101 0.048(2) 0.047(2) 0.098(3) 0.002(2) 0.063(2) 0.0011(18) N101 0.0236(19) 0.0209(19) 0.036(2) -0.0006(16) 0.0186(18) 0.0014(15) O102 0.043(2) 0.0241(18) 0.064(3) -0.0064(17) 0.033(2) -0.0045(15) N102 0.024(2) 0.032(2) 0.039(2) -0.0034(18) 0.0215(19) -0.0026(17) O103 0.044(2) 0.0248(19) 0.062(3) -0.0036(17) 0.016(2) -0.0029(16) N103 0.031(3) 0.028(3) 0.040(3) 0.000 0.022(3) 0.000 O104 0.045(2) 0.055(2) 0.101(3) -0.002(2) 0.063(3) 0.0019(19) O105 0.036(2) 0.043(2) 0.079(3) 0.0074(19) 0.048(2) 0.0003(16) O106 0.034(2) 0.051(2) 0.078(3) 0.000(2) 0.046(2) 0.0006(17) O107 0.044(2) 0.0321(19) 0.063(3) -0.0156(18) 0.030(2) -0.0117(16) O108 0.0355(19) 0.042(2) 0.067(3) -0.0119(18) 0.042(2) -0.0130(16) Ag3A 0.0617(8) 0.0287(6) 0.0790(9) -0.0117(6) 0.0568(8) -0.0139(5) Ag4A 0.072(4) 0.010(2) 0.113(6) -0.009(2) 0.082(4) -0.007(2) O22A 0.064(6) 0.025(4) 0.015(4) 0.002(3) 0.026(4) -0.001(4) C20M 0.063(4) 0.042(3) 0.049(4) -0.002(3) 0.037(3) 0.006(3) C21M 0.084(6) 0.024(4) 0.070(6) 0.000 0.055(5) 0.000 C22M 0.059(4) 0.039(3) 0.045(4) 0.006(3) 0.025(3) 0.010(3) C23M 0.053(3) 0.026(3) 0.042(3) 0.001(2) 0.029(3) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.212(4) . ? Ag1 N1 2.233(4) . ? Ag1 O20 2.370(4) . ? O1 C8 1.223(5) . ? N1 C13 1.324(6) . ? N1 C12 1.345(5) . ? C1 C2 1.505(6) . ? Ag2 Ag2 1.5764(19) 2 ? Ag2 N7 2.241(4) 2 ? Ag2 O21 2.285(7) . ? Ag2 N7 2.396(5) . ? Ag2 O21 2.440(7) 2 ? Ag2 O2 2.532(3) . ? O2 C19 1.227(5) . ? N2 C8 1.377(6) . ? N2 C9 1.403(6) . ? C2 C3 1.386(6) . ? C2 C7 1.395(6) . ? Ag3 N10 2.158(5) . ? Ag3 N13 2.196(4) . ? Ag3 O22 2.333(8) . ? O3 C34 1.225(5) . ? N3 C8 1.375(6) . ? N3 C5 1.408(6) . ? C3 C4 1.379(6) . ? Ag4 N16 2.257(4) . ? Ag4 N19 2.268(4) . ? Ag4 O23 2.447(4) . ? O4 C47 1.233(6) . ? N4 C18 1.324(5) . ? N4 C14 1.341(5) . ? C4 C5 1.393(6) . ? O5 C58 1.241(5) . ? N5 C19 1.377(5) . ? N5 C17 1.397(5) . ? C5 C6 1.392(6) . ? O6 C73 1.234(5) . ? N6 C19 1.354(6) . ? N6 C20 1.419(5) . ? C6 C7 1.385(7) . ? O7 C84 1.240(5) . ? N7 C39 1.321(7) . ? N7 C38 1.331(7) . ? N7 Ag2 2.241(4) 2 ? N8 C34 1.377(6) . ? N8 C35 1.391(6) . ? N9 C34 1.363(6) . ? N9 C31 1.407(6) . ? C9 C10 1.389(6) . ? C9 C13 1.398(6) . ? N10 C52 1.333(7) . ? N10 C51 1.337(6) . ? N10 Ag3A 2.372(5) . ? C10 C11 1.391(7) . ? N11 C47 1.377(7) . ? N11 C48 1.410(7) . ? C11 C12 1.390(6) . ? N12 C47 1.346(7) . ? N12 C44 1.415(7) . ? N13 C53 1.330(6) . ? N13 C57 1.338(6) . ? N13 Ag3A 2.283(4) . ? N14 C58 1.376(5) . ? N14 C54 1.402(6) . ? C14 C15 1.379(6) . ? N15 C58 1.342(6) . ? N15 C59 1.421(5) . ? C15 C16 1.378(6) . ? N16 C78 1.330(6) . ? N16 C77 1.340(6) . ? N16 Ag4A 2.343(6) . ? C16 C17 1.390(6) . ? N17 C73 1.376(5) . ? N17 C74 1.394(5) . ? C17 C18 1.395(6) . ? N18 C73 1.351(5) . ? N18 C70 1.410(5) . ? N19 C79 1.332(6) . ? N19 C83 1.333(6) . ? N19 Ag4A 2.296(6) . ? O20 C20M 1.414(6) . ? N20 C84 1.375(6) . ? N20 C80 1.394(6) . ? C20 C21 1.379(6) . ? C20 C25 1.390(6) . ? O21 C21M 1.403(9) . ? O21 O21 1.432(14) 2 ? O21 Ag2 2.440(7) 2 ? N21 C84 1.354(6) . ? N21 C85 1.417(6) . ? C21 C22 1.387(6) . ? O22 C22M 1.470(10) . ? C22 C23 1.389(6) . ? O23 C23M 1.420(6) . ? C23 C24 1.384(6) . ? C23 C26 1.506(6) . ? O24 N103 1.231(8) . ? C24 C25 1.388(6) . ? O25 N103 1.238(4) . ? C27 C28 1.506(7) . ? C28 C33 1.392(6) . ? C28 C29 1.397(6) . ? C29 C30 1.390(6) . ? C30 C31 1.400(6) . ? C31 C32 1.386(7) . ? C32 C33 1.377(7) . ? C35 C39 1.374(7) . ? C35 C36 1.390(6) . ? C36 C37 1.382(7) . ? C37 C38 1.371(7) . ? C40 C41 1.499(8) . ? C41 C42 1.379(7) . ? C41 C46 1.386(7) . ? C42 C43 1.388(8) . ? C43 C44 1.397(6) . ? C44 C45 1.376(7) . ? C45 C46 1.392(8) . ? C48 C52 1.386(7) . ? C48 C49 1.388(6) . ? C49 C50 1.394(9) . ? C50 C51 1.382(8) . ? C53 C54 1.390(6) . ? C54 C55 1.393(6) . ? C55 C56 1.386(6) . ? C56 C57 1.379(7) . ? C59 C60 1.387(6) . ? C59 C64 1.392(6) . ? C60 C61 1.390(6) . ? C61 C62 1.396(6) . ? C62 C63 1.372(7) . ? C62 C65 1.511(6) . ? C63 C64 1.391(7) . ? C66 C67 1.497(6) . ? C67 C68 1.389(6) . ? C67 C72 1.392(6) . ? C68 C69 1.389(6) . ? C69 C70 1.393(5) . ? C70 C71 1.393(6) . ? C71 C72 1.381(6) . ? C74 C78 1.394(6) . ? C74 C75 1.401(6) . ? C75 C76 1.382(6) . ? C76 C77 1.370(6) . ? C79 C80 1.390(6) . ? C80 C81 1.400(6) . ? C81 C82 1.367(7) . ? C82 C83 1.388(7) . ? C85 C90 1.382(6) . ? C85 C86 1.389(6) . ? C86 C87 1.376(7) . ? C87 C88 1.396(6) . ? C88 C89 1.383(7) . ? C88 C91 1.509(7) . ? C89 C90 1.386(7) . ? O100 N100 1.240(5) . ? N100 O101 1.231(5) . ? N100 O102 1.253(5) . ? N101 O104 1.222(5) . ? N101 O105 1.243(5) . ? N101 O103 1.246(5) . ? N102 O106 1.241(5) . ? N102 O107 1.241(5) . ? N102 O108 1.245(5) . ? N103 O25 1.238(4) 2 ? Ag3A O22A 2.391(8) . ? Ag4A O23A 2.13(5) . ? O22A C22M 1.376(9) . ? C21M O21 1.403(9) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N1 130.51(13) . . ? N4 Ag1 O20 120.14(14) . . ? N1 Ag1 O20 103.57(14) . . ? C13 N1 C12 119.0(4) . . ? C13 N1 Ag1 121.1(3) . . ? C12 N1 Ag1 119.7(3) . . ? Ag2 Ag2 N7 75.54(16) 2 2 ? Ag2 Ag2 O21 75.89(19) 2 . ? N7 Ag2 O21 124.7(2) 2 . ? Ag2 Ag2 N7 64.89(14) 2 . ? N7 Ag2 N7 118.28(19) 2 . ? O21 Ag2 N7 89.8(2) . . ? Ag2 Ag2 O21 65.31(18) 2 2 ? N7 Ag2 O21 89.7(2) 2 2 ? O21 Ag2 O21 35.1(3) . 2 ? N7 Ag2 O21 112.0(2) . 2 ? Ag2 Ag2 O2 143.42(9) 2 . ? N7 Ag2 O2 137.34(17) 2 . ? O21 Ag2 O2 71.1(2) . . ? N7 Ag2 O2 99.32(15) . . ? O21 Ag2 O2 94.41(18) 2 . ? C19 O2 Ag2 114.5(3) . . ? C8 N2 C9 125.9(4) . . ? C3 C2 C7 117.0(4) . . ? C3 C2 C1 121.2(4) . . ? C7 C2 C1 121.9(4) . . ? N10 Ag3 N13 133.45(16) . . ? N10 Ag3 O22 101.0(2) . . ? N13 Ag3 O22 118.0(2) . . ? C8 N3 C5 125.3(4) . . ? C4 C3 C2 122.2(4) . . ? N16 Ag4 N19 122.14(14) . . ? N16 Ag4 O23 92.11(13) . . ? N19 Ag4 O23 113.79(14) . . ? C18 N4 C14 118.8(4) . . ? C18 N4 Ag1 114.6(3) . . ? C14 N4 Ag1 124.8(3) . . ? C3 C4 C5 119.9(4) . . ? C19 N5 C17 126.6(4) . . ? C6 C5 C4 119.2(4) . . ? C6 C5 N3 117.7(4) . . ? C4 C5 N3 123.0(4) . . ? C19 N6 C20 126.8(4) . . ? C7 C6 C5 119.6(4) . . ? C39 N7 C38 119.1(4) . . ? C39 N7 Ag2 118.0(4) . 2 ? C38 N7 Ag2 122.2(4) . 2 ? C39 N7 Ag2 114.8(3) . . ? C38 N7 Ag2 116.5(4) . . ? Ag2 N7 Ag2 39.57(9) 2 . ? C6 C7 C2 122.1(4) . . ? C34 N8 C35 126.4(4) . . ? O1 C8 N3 123.4(4) . . ? O1 C8 N2 123.8(4) . . ? N3 C8 N2 112.7(4) . . ? C34 N9 C31 127.3(4) . . ? C10 C9 C13 118.1(4) . . ? C10 C9 N2 125.0(4) . . ? C13 C9 N2 116.9(4) . . ? C52 N10 C51 118.4(5) . . ? C52 N10 Ag3 118.7(3) . . ? C51 N10 Ag3 122.9(4) . . ? C52 N10 Ag3A 122.1(3) . . ? C51 N10 Ag3A 115.5(4) . . ? Ag3 N10 Ag3A 22.35(6) . . ? C9 C10 C11 118.2(4) . . ? C47 N11 C48 126.2(4) . . ? C12 C11 C10 120.2(4) . . ? C47 N12 C44 127.0(4) . . ? N1 C12 C11 121.0(4) . . ? C53 N13 C57 118.2(4) . . ? C53 N13 Ag3 112.9(3) . . ? C57 N13 Ag3 124.8(3) . . ? C53 N13 Ag3A 119.4(3) . . ? C57 N13 Ag3A 122.3(3) . . ? Ag3 N13 Ag3A 23.15(5) . . ? N1 C13 C9 123.4(4) . . ? C58 N14 C54 126.8(4) . . ? N4 C14 C15 121.4(4) . . ? C58 N15 C59 127.6(4) . . ? C16 C15 C14 120.3(4) . . ? C78 N16 C77 118.6(4) . . ? C78 N16 Ag4 120.6(3) . . ? C77 N16 Ag4 120.6(3) . . ? C78 N16 Ag4A 116.0(3) . . ? C77 N16 Ag4A 110.6(3) . . ? Ag4 N16 Ag4A 35.91(16) . . ? C15 C16 C17 118.4(4) . . ? C73 N17 C74 126.6(4) . . ? C16 C17 C18 117.8(4) . . ? C16 C17 N5 126.1(4) . . ? C18 C17 N5 116.0(4) . . ? C73 N18 C70 127.9(3) . . ? N4 C18 C17 123.3(4) . . ? C79 N19 C83 118.4(4) . . ? C79 N19 Ag4 116.5(3) . . ? C83 N19 Ag4 122.0(3) . . ? C79 N19 Ag4A 113.2(3) . . ? C83 N19 Ag4A 124.8(4) . . ? Ag4 N19 Ag4A 36.27(18) . . ? O2 C19 N6 124.9(4) . . ? O2 C19 N5 122.8(4) . . ? N6 C19 N5 112.3(4) . . ? C20M O20 Ag1 126.4(3) . . ? C84 N20 C80 126.1(4) . . ? C21 C20 C25 118.6(4) . . ? C21 C20 N6 117.6(4) . . ? C25 C20 N6 123.8(4) . . ? C21M O21 O21 59.3(3) . 2 ? C21M O21 Ag2 133.7(5) . . ? O21 O21 Ag2 78.3(3) 2 . ? C21M O21 Ag2 122.7(4) . 2 ? O21 O21 Ag2 66.6(2) 2 2 ? Ag2 O21 Ag2 38.80(12) . 2 ? C84 N21 C85 126.9(4) . . ? C20 C21 C22 121.0(4) . . ? C22M O22 Ag3 132.8(6) . . ? C21 C22 C23 121.1(4) . . ? C23M O23 Ag4 123.6(3) . . ? C24 C23 C22 117.5(4) . . ? C24 C23 C26 121.2(4) . . ? C22 C23 C26 121.3(4) . . ? C23 C24 C25 121.9(4) . . ? C24 C25 C20 120.0(4) . . ? C33 C28 C29 116.8(4) . . ? C33 C28 C27 121.7(4) . . ? C29 C28 C27 121.5(4) . . ? C30 C29 C28 121.8(4) . . ? C29 C30 C31 120.0(4) . . ? C32 C31 C30 118.6(4) . . ? C32 C31 N9 117.2(4) . . ? C30 C31 N9 124.2(4) . . ? C33 C32 C31 120.6(4) . . ? C32 C33 C28 122.2(4) . . ? O3 C34 N9 124.4(4) . . ? O3 C34 N8 122.4(4) . . ? N9 C34 N8 113.2(4) . . ? C39 C35 C36 117.1(5) . . ? C39 C35 N8 117.1(4) . . ? C36 C35 N8 125.8(4) . . ? C37 C36 C35 119.0(4) . . ? C38 C37 C36 119.7(5) . . ? N7 C38 C37 121.2(5) . . ? N7 C39 C35 123.9(5) . . ? C42 C41 C46 117.5(5) . . ? C42 C41 C40 121.0(5) . . ? C46 C41 C40 121.5(5) . . ? C41 C42 C43 122.3(5) . . ? C42 C43 C44 119.2(5) . . ? C45 C44 C43 119.4(5) . . ? C45 C44 N12 117.9(4) . . ? C43 C44 N12 122.7(5) . . ? C44 C45 C46 120.2(4) . . ? C41 C46 C45 121.4(5) . . ? O4 C47 N12 123.2(5) . . ? O4 C47 N11 122.8(5) . . ? N12 C47 N11 114.0(4) . . ? C52 C48 C49 118.2(5) . . ? C52 C48 N11 117.3(4) . . ? C49 C48 N11 124.6(5) . . ? C48 C49 C50 118.2(5) . . ? C51 C50 C49 119.7(5) . . ? N10 C51 C50 122.0(6) . . ? N10 C52 C48 123.6(4) . . ? N13 C53 C54 124.1(4) . . ? C53 C54 C55 117.6(4) . . ? C53 C54 N14 116.2(4) . . ? C55 C54 N14 126.2(4) . . ? C56 C55 C54 118.1(4) . . ? C57 C56 C55 120.5(4) . . ? N13 C57 C56 121.6(4) . . ? O5 C58 N15 124.8(4) . . ? O5 C58 N14 122.1(4) . . ? N15 C58 N14 113.0(4) . . ? C60 C59 C64 119.1(4) . . ? C60 C59 N15 116.7(4) . . ? C64 C59 N15 124.2(4) . . ? C59 C60 C61 120.1(4) . . ? C60 C61 C62 121.3(4) . . ? C63 C62 C61 117.6(4) . . ? C63 C62 C65 121.5(4) . . ? C61 C62 C65 120.9(4) . . ? C62 C63 C64 122.3(4) . . ? C63 C64 C59 119.6(4) . . ? C68 C67 C72 116.3(4) . . ? C68 C67 C66 121.9(4) . . ? C72 C67 C66 121.8(4) . . ? C67 C68 C69 122.8(4) . . ? C68 C69 C70 119.5(4) . . ? C69 C70 C71 118.7(4) . . ? C69 C70 N18 124.3(4) . . ? C71 C70 N18 117.0(4) . . ? C72 C71 C70 120.3(4) . . ? C71 C72 C67 122.3(4) . . ? O6 C73 N18 124.1(4) . . ? O6 C73 N17 122.2(4) . . ? N18 C73 N17 113.7(4) . . ? C78 C74 N17 117.1(4) . . ? C78 C74 C75 117.4(4) . . ? N17 C74 C75 125.5(4) . . ? C76 C75 C74 118.4(4) . . ? C77 C76 C75 120.4(4) . . ? N16 C77 C76 121.8(4) . . ? N16 C78 C74 123.5(4) . . ? N19 C79 C80 123.9(4) . . ? C79 C80 N20 116.9(4) . . ? C79 C80 C81 117.2(4) . . ? N20 C80 C81 125.9(4) . . ? C82 C81 C80 118.6(4) . . ? C81 C82 C83 120.5(4) . . ? N19 C83 C82 121.4(5) . . ? O7 C84 N21 124.2(4) . . ? O7 C84 N20 122.2(4) . . ? N21 C84 N20 113.6(4) . . ? C90 C85 C86 118.7(4) . . ? C90 C85 N21 124.8(4) . . ? C86 C85 N21 116.5(4) . . ? C87 C86 C85 120.7(4) . . ? C86 C87 C88 121.7(4) . . ? C89 C88 C87 116.6(4) . . ? C89 C88 C91 121.8(4) . . ? C87 C88 C91 121.5(4) . . ? C88 C89 C90 122.5(4) . . ? C85 C90 C89 119.8(4) . . ? O101 N100 O100 119.9(4) . . ? O101 N100 O102 120.9(4) . . ? O100 N100 O102 119.2(4) . . ? O104 N101 O105 119.6(4) . . ? O104 N101 O103 122.1(4) . . ? O105 N101 O103 118.3(4) . . ? O106 N102 O107 121.1(4) . . ? O106 N102 O108 119.5(4) . . ? O107 N102 O108 119.4(4) . . ? O24 N103 O25 120.8(3) . 2 ? O24 N103 O25 120.8(3) . . ? O25 N103 O25 118.5(6) 2 . ? N13 Ag3A N10 118.43(16) . . ? N13 Ag3A O22A 104.1(2) . . ? N10 Ag3A O22A 105.3(2) . . ? O23A Ag4A N19 97.6(15) . . ? O23A Ag4A N16 115.0(14) . . ? N19 Ag4A N16 117.3(3) . . ? C22M O22A Ag3A 120.9(5) . . ? O21 C21M O21 61.4(7) 2 . ? O22A C22M O22 40.8(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O101 0.88 2.16 2.965(5) 152.3 . N3 H3B O101 0.88 2.17 2.929(5) 143.7 . N5 H5A O102 0.88 2.08 2.931(5) 162.7 . N6 H6B O100 0.88 2.06 2.935(5) 173.6 . N8 H8A O24 0.88 2.42 3.274(4) 163.4 . N8 H8A O25 0.88 2.59 3.350(5) 144.9 . N9 H9A O25 0.88 1.99 2.864(5) 175.8 . N11 H11B O106 0.88 2.21 2.990(5) 147.3 . N12 H12B O106 0.88 2.16 2.922(5) 145.3 . N14 H14B O107 0.88 2.10 2.959(5) 164.1 . N15 H15B O108 0.88 2.05 2.927(5) 178.9 . N17 H17A O104 0.88 2.33 3.118(5) 149.1 . N18 H18B O104 0.88 1.99 2.851(5) 167.2 . N20 H20A O103 0.88 2.14 2.975(5) 157.9 . N21 H21B O105 0.88 2.01 2.878(5) 171.0 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.909 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.135 data_C:\structs\JWS\Dave\dtag018\DTAG018.CIF _database_code_depnum_ccdc_archive 'CCDC 233239' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common dtag018 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H26.67 Ag F3 N6 O5.33 S' _chemical_formula_weight 717.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1774(5) _cell_length_b 16.7930(15) _cell_length_c 19.6054(18) _cell_angle_alpha 107.586(3) _cell_angle_beta 93.998(3) _cell_angle_gamma 91.066(4) _cell_volume 2245.2(3) _cell_formula_units_Z 3 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blade _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1090 _exptl_absorpt_coefficient_mu 0.810 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7931 _exptl_absorpt_correction_T_max 0.9606 _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program Scalepack Z. Otwinowski and W. Minor, in Methods in Enzymology, ed. C. W. Carter and R. M. Sweet, Academic Press: London, 1997, vol. 276, pp 307. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 0.71 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 7417 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.96 _reflns_number_total 5223 _reflns_number_gt 3996 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0281P)^2^+6.8193P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(8) _refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5223 _refine_ls_number_parameters 660 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.53801(8) 0.84366(4) 0.31437(3) 0.0386(3) Uani 1 1 d . . . Ag2 Ag 0.5000 0.5000 0.0000 0.0371(3) Uani 1 2 d S . . S1 S 0.2243(4) 0.30810(15) 0.29678(15) 0.0569(7) Uani 1 1 d . . . S2 S 0.8805(6) -0.0190(3) -0.0240(3) 0.0537(13) Uani 0.50 1 d P . 1 F1 F 0.4923(12) 0.2722(7) 0.3791(5) 0.155(4) Uani 1 1 d . . . F2 F 0.5462(11) 0.2407(7) 0.2719(5) 0.152(4) Uani 1 1 d . . . F3 F 0.5632(11) 0.3667(6) 0.3361(7) 0.199(6) Uani 1 1 d . . . F4 F 0.6432(17) -0.1151(8) -0.1112(6) 0.084(4) Uani 0.50 1 d PU A 1 F5 F 0.5311(16) -0.0011(9) -0.0584(8) 0.103(5) Uani 0.50 1 d P A 1 F6 F 0.5752(17) -0.0892(8) 0.0006(8) 0.096(4) Uani 0.50 1 d P A 1 O1 O 0.8165(7) 1.1488(3) 0.4661(3) 0.0435(14) Uani 1 1 d . . . O2 O 0.3448(7) 0.5496(3) 0.1425(3) 0.0426(14) Uani 1 1 d . . . O3 O 0.6824(6) 0.2141(3) -0.1808(3) 0.0330(12) Uani 1 1 d . . . O4 O 0.1586(15) 0.3599(7) 0.3654(6) 0.080(5) Uani 0.73(2) 1 d P B 1 O5 O 0.1490(16) 0.2231(7) 0.2791(8) 0.067(4) Uani 0.73(2) 1 d P B 1 O6 O 0.2280(18) 0.3428(10) 0.2433(7) 0.098(5) Uani 0.73(2) 1 d P B 1 O8 O 0.8608(16) 0.0485(7) 0.0407(8) 0.062(4) Uani 0.50 1 d P . 1 O9 O 0.9800(18) -0.0876(7) -0.0116(7) 0.064(4) Uani 0.50 1 d P . 1 N1 N 0.6676(8) 0.9433(4) 0.2837(4) 0.0354(16) Uani 1 1 d . . . N2 N 0.8763(8) 1.1576(4) 0.3552(4) 0.0372(16) Uani 1 1 d . . . H2 H 0.9235 1.1920 0.3342 0.045 Uiso 1 1 calc R . . N3 N 0.9814(9) 1.2621(4) 0.4538(4) 0.0405(17) Uani 1 1 d . . . H3 H 1.0233 1.2827 0.4211 0.049 Uiso 1 1 calc R . . N4 N 0.4617(8) 0.7327(4) 0.3405(4) 0.0356(16) Uani 1 1 d . . . N5 N 0.3074(8) 0.5134(4) 0.2442(4) 0.0342(16) Uani 1 1 d . . . H5 H 0.2735 0.4713 0.2593 0.041 Uiso 1 1 calc R . . N6 N 0.2252(8) 0.4183(4) 0.1350(3) 0.0339(16) Uani 1 1 d . . . H6 H 0.1884 0.3870 0.1607 0.041 Uiso 1 1 calc R . . N7 N 0.6457(7) 0.3921(3) 0.0176(3) 0.0280(15) Uani 1 1 d . . . N8 N 0.7765(8) 0.1783(4) -0.0803(3) 0.0345(16) Uani 1 1 d . . . H8 H 0.8215 0.1369 -0.0662 0.041 Uiso 1 1 calc R . . N9 N 0.8117(8) 0.0873(4) -0.1918(4) 0.0363(16) Uani 1 1 d . . . H9 H 0.8644 0.0565 -0.1673 0.044 Uiso 1 1 calc R . . C1 C 0.6705(10) 0.9329(5) 0.2134(5) 0.036(2) Uani 1 1 d . . . H1 H 0.6235 0.8815 0.1800 0.043 Uiso 1 1 calc R . . C2 C 0.7390(10) 0.9938(5) 0.1887(5) 0.038(2) Uani 1 1 d . . . H2A H 0.7398 0.9848 0.1385 0.046 Uiso 1 1 calc R . . C3 C 0.8075(10) 1.0687(5) 0.2362(5) 0.040(2) Uani 1 1 d . . . H3A H 0.8579 1.1112 0.2192 0.047 Uiso 1 1 calc R . . C4 C 0.8020(10) 1.0813(5) 0.3094(5) 0.0319(19) Uani 1 1 d . . . C5 C 0.7317(9) 1.0160(5) 0.3310(5) 0.0340(19) Uani 1 1 d . . . H5A H 0.7289 1.0231 0.3808 0.041 Uiso 1 1 calc R . . C6 C 0.8852(10) 1.1857(5) 0.4285(5) 0.035(2) Uani 1 1 d . . . C7 C 1.0205(9) 1.3116(5) 0.5266(4) 0.036(2) Uani 1 1 d . . . C8 C 1.0667(10) 1.3968(5) 0.5393(5) 0.046(2) Uani 1 1 d . . . H8A H 1.0673 1.4193 0.5003 0.055 Uiso 1 1 calc R . . C9 C 1.1114(10) 1.4479(5) 0.6089(5) 0.050(3) Uani 1 1 d . . . H9A H 1.1385 1.5057 0.6167 0.060 Uiso 1 1 calc R . . C10 C 1.1181(10) 1.4182(6) 0.6668(5) 0.048(2) Uani 1 1 d . . . C11 C 1.0728(10) 1.3330(6) 0.6526(5) 0.045(2) Uani 1 1 d . . . H11 H 1.0749 1.3106 0.6917 0.053 Uiso 1 1 calc R . . C12 C 1.0252(10) 1.2804(5) 0.5844(5) 0.039(2) Uani 1 1 d . . . H12 H 0.9956 1.2229 0.5771 0.047 Uiso 1 1 calc R . . C13 C 1.1726(12) 1.4747(6) 0.7410(5) 0.068(3) Uani 1 1 d . . . H13A H 1.3092 1.4793 0.7492 0.102 Uiso 1 1 calc R . . H13B H 1.1201 1.4516 0.7761 0.102 Uiso 1 1 calc R . . H13C H 1.1242 1.5303 0.7461 0.102 Uiso 1 1 calc R . . C14 C 0.4726(10) 0.7292(5) 0.4085(4) 0.039(2) Uani 1 1 d . . . H14 H 0.5084 0.7782 0.4469 0.046 Uiso 1 1 calc R . . C15 C 0.4330(10) 0.6563(5) 0.4229(5) 0.039(2) Uani 1 1 d . . . H15 H 0.4421 0.6553 0.4712 0.047 Uiso 1 1 calc R . . C16 C 0.3803(10) 0.5847(5) 0.3685(5) 0.037(2) Uani 1 1 d . . . H16 H 0.3538 0.5341 0.3788 0.044 Uiso 1 1 calc R . . C17 C 0.3660(9) 0.5870(5) 0.2979(4) 0.0326(19) Uani 1 1 d . . . C18 C 0.4069(9) 0.6626(5) 0.2857(4) 0.0321(19) Uani 1 1 d . . . H18 H 0.3963 0.6654 0.2379 0.038 Uiso 1 1 calc R . . C19 C 0.2955(9) 0.4977(5) 0.1716(4) 0.0313(19) Uani 1 1 d . . . C20 C 0.2073(9) 0.3832(4) 0.0599(4) 0.0301(18) Uani 1 1 d . . . C21 C 0.2348(9) 0.2975(5) 0.0302(5) 0.038(2) Uani 1 1 d . . . H21 H 0.2657 0.2642 0.0605 0.046 Uiso 1 1 calc R . . C22 C 0.2164(9) 0.2615(5) -0.0441(4) 0.034(2) Uani 1 1 d . . . H22 H 0.2342 0.2034 -0.0639 0.041 Uiso 1 1 calc R . . C23 C 0.1724(9) 0.3089(5) -0.0903(4) 0.034(2) Uani 1 1 d . . . C24 C 0.1417(9) 0.3929(5) -0.0591(4) 0.0323(19) Uani 1 1 d . . . H24 H 0.1083 0.4261 -0.0892 0.039 Uiso 1 1 calc R . . C25 C 0.1582(9) 0.4300(4) 0.0147(4) 0.0313(19) Uani 1 1 d . . . H25 H 0.1357 0.4877 0.0343 0.038 Uiso 1 1 calc R . . C26 C 0.1569(11) 0.2695(5) -0.1696(4) 0.045(2) Uani 1 1 d . . . H26A H 0.2775 0.2756 -0.1885 0.068 Uiso 1 1 calc R . . H26B H 0.0612 0.2969 -0.1916 0.068 Uiso 1 1 calc R . . H26C H 0.1218 0.2100 -0.1809 0.068 Uiso 1 1 calc R . . C27 C 0.6777(9) 0.3901(5) 0.0853(4) 0.0347(19) Uani 1 1 d . . . H27 H 0.6572 0.4386 0.1238 0.042 Uiso 1 1 calc R . . C28 C 0.7396(10) 0.3196(5) 0.1005(4) 0.038(2) Uani 1 1 d . . . H28 H 0.7615 0.3195 0.1488 0.046 Uiso 1 1 calc R . . C29 C 0.7695(10) 0.2489(5) 0.0441(4) 0.0343(19) Uani 1 1 d . . . H29 H 0.8105 0.1995 0.0535 0.041 Uiso 1 1 calc R . . C30 C 0.7392(9) 0.2508(4) -0.0259(4) 0.0307(18) Uani 1 1 d . . . C31 C 0.6789(9) 0.3245(4) -0.0372(4) 0.0293(18) Uani 1 1 d . . . H31 H 0.6608 0.3270 -0.0850 0.035 Uiso 1 1 calc R . . C32 C 0.7510(9) 0.1641(4) -0.1535(4) 0.0291(18) Uani 1 1 d . . . C33 C 0.7960(9) 0.0546(5) -0.2667(4) 0.033(2) Uani 1 1 d . . . C34 C 0.7474(10) -0.0303(5) -0.2981(5) 0.037(2) Uani 1 1 d . . . H34 H 0.7266 -0.0642 -0.2681 0.044 Uiso 1 1 calc R . . C35 C 0.7293(10) -0.0656(5) -0.3711(5) 0.037(2) Uani 1 1 d . . . H35 H 0.6973 -0.1236 -0.3909 0.045 Uiso 1 1 calc R . . C36 C 0.7570(10) -0.0182(5) -0.4167(4) 0.038(2) Uani 1 1 d . . . C37 C 0.8087(9) 0.0663(5) -0.3863(4) 0.0352(19) Uani 1 1 d . . . H37 H 0.8310 0.0995 -0.4167 0.042 Uiso 1 1 calc R . . C38 C 0.8282(9) 0.1026(5) -0.3122(5) 0.036(2) Uani 1 1 d . . . H38 H 0.8635 0.1602 -0.2925 0.044 Uiso 1 1 calc R . . C39 C 0.7383(12) -0.0567(5) -0.4971(4) 0.051(2) Uani 1 1 d . . . H39A H 0.7888 -0.1127 -0.5097 0.076 Uiso 1 1 calc R . . H39B H 0.8079 -0.0217 -0.5193 0.076 Uiso 1 1 calc R . . H39C H 0.6061 -0.0609 -0.5146 0.076 Uiso 1 1 calc R . . C40 C 0.4721(18) 0.2972(8) 0.3183(9) 0.092(4) Uani 1 1 d . B . C41 C 0.648(3) -0.0653(13) -0.0567(16) 0.075(7) Uani 0.50 1 d P A 1 O7 O 0.925(2) 0.0091(13) -0.0844(9) 0.099(6) Uani 0.50 1 d P C 1 O1S O 0.811(2) -0.0501(10) -0.1295(9) 0.082(5) Uani 0.50 1 d P D 2 O4A O 0.205(3) 0.3974(13) 0.3243(13) 0.045(9) Uani 0.27(2) 1 d PU B 2 O6A O 0.213(4) 0.288(2) 0.2072(17) 0.063(9) Uani 0.27(2) 1 d PU B 2 O5A O 0.128(5) 0.253(2) 0.314(2) 0.072(12) Uani 0.27(2) 1 d PU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0400(4) 0.0318(4) 0.0410(5) 0.0072(3) 0.0011(3) -0.0004(3) Ag2 0.0374(5) 0.0268(5) 0.0457(6) 0.0087(5) 0.0018(4) 0.0091(4) S1 0.0737(16) 0.0381(13) 0.0576(18) 0.0139(15) 0.0013(13) -0.0053(12) S2 0.061(3) 0.050(3) 0.062(3) 0.031(3) 0.012(2) 0.025(2) F1 0.127(7) 0.203(10) 0.117(7) 0.033(7) -0.038(5) 0.040(6) F2 0.118(6) 0.192(9) 0.131(7) 0.017(7) 0.032(5) 0.068(6) F3 0.098(6) 0.108(7) 0.367(17) 0.055(9) -0.052(8) -0.057(5) F4 0.103(7) 0.081(7) 0.042(6) -0.014(6) -0.021(6) 0.002(6) F5 0.060(7) 0.122(11) 0.134(12) 0.059(10) -0.031(7) 0.007(7) F6 0.080(8) 0.098(10) 0.121(11) 0.056(10) -0.021(8) -0.029(7) O1 0.051(3) 0.039(3) 0.041(4) 0.012(3) 0.008(3) -0.006(3) O2 0.055(3) 0.033(3) 0.040(4) 0.013(3) 0.002(3) -0.007(3) O3 0.036(3) 0.029(3) 0.032(3) 0.008(3) 0.000(2) 0.008(2) O4 0.109(8) 0.065(7) 0.053(8) -0.005(6) 0.002(6) 0.022(6) O5 0.090(8) 0.040(6) 0.079(10) 0.029(7) 0.022(7) -0.006(5) O6 0.152(11) 0.089(11) 0.068(10) 0.057(10) -0.019(7) -0.041(8) O8 0.052(7) 0.034(6) 0.094(11) 0.013(8) -0.002(7) 0.011(6) O9 0.078(9) 0.048(7) 0.071(9) 0.026(7) -0.003(7) 0.032(7) N1 0.028(3) 0.030(4) 0.043(5) 0.002(4) 0.000(3) -0.002(3) N2 0.044(4) 0.032(4) 0.033(5) 0.006(4) 0.001(3) -0.001(3) N3 0.052(4) 0.038(4) 0.031(5) 0.009(4) 0.005(3) -0.003(3) N4 0.028(3) 0.030(4) 0.041(5) -0.001(4) 0.000(3) -0.002(3) N5 0.042(4) 0.025(4) 0.034(5) 0.007(4) -0.001(3) -0.003(3) N6 0.038(4) 0.029(4) 0.033(4) 0.007(4) 0.006(3) -0.004(3) N7 0.026(3) 0.027(3) 0.031(4) 0.007(3) 0.004(3) 0.005(3) N8 0.044(4) 0.024(3) 0.033(4) 0.005(3) -0.002(3) 0.011(3) N9 0.043(4) 0.030(4) 0.036(5) 0.010(4) 0.003(3) 0.013(3) C1 0.032(4) 0.038(5) 0.030(5) 0.000(4) -0.001(4) 0.007(4) C2 0.042(5) 0.041(5) 0.035(5) 0.017(5) -0.002(4) 0.001(4) C3 0.043(5) 0.033(5) 0.038(6) 0.004(5) 0.000(4) -0.002(4) C4 0.030(4) 0.028(4) 0.037(6) 0.009(5) 0.002(4) 0.008(3) C5 0.029(4) 0.037(5) 0.031(5) 0.003(5) 0.002(4) 0.004(4) C6 0.034(4) 0.023(4) 0.040(6) -0.004(5) 0.001(4) 0.009(4) C7 0.028(4) 0.034(5) 0.034(6) -0.003(5) -0.005(4) -0.001(3) C8 0.041(5) 0.038(5) 0.054(7) 0.011(5) -0.002(4) -0.001(4) C9 0.037(5) 0.036(5) 0.057(7) -0.012(6) -0.007(5) 0.001(4) C10 0.029(4) 0.057(6) 0.046(6) 0.000(6) -0.006(4) 0.008(4) C11 0.039(5) 0.057(6) 0.032(6) 0.005(5) 0.002(4) 0.012(4) C12 0.038(4) 0.036(5) 0.038(6) 0.007(5) -0.001(4) 0.005(4) C13 0.041(5) 0.080(7) 0.057(7) -0.017(6) 0.001(5) 0.003(5) C14 0.039(4) 0.048(5) 0.027(5) 0.008(5) 0.004(4) 0.001(4) C15 0.043(5) 0.045(5) 0.033(5) 0.016(5) 0.004(4) 0.001(4) C16 0.035(4) 0.036(5) 0.043(6) 0.017(5) 0.007(4) 0.005(4) C17 0.029(4) 0.033(5) 0.038(6) 0.013(5) 0.004(4) 0.008(3) C18 0.031(4) 0.035(5) 0.029(5) 0.007(5) 0.003(4) 0.006(3) C19 0.026(4) 0.029(5) 0.034(6) 0.002(5) 0.003(4) 0.000(3) C20 0.029(4) 0.025(4) 0.036(5) 0.008(4) 0.004(4) 0.007(3) C21 0.031(4) 0.032(4) 0.056(7) 0.019(5) 0.005(4) 0.000(3) C22 0.032(4) 0.029(4) 0.040(6) 0.006(5) 0.006(4) 0.003(3) C23 0.026(4) 0.035(4) 0.038(5) 0.007(5) 0.002(4) -0.003(3) C24 0.028(4) 0.033(4) 0.034(5) 0.007(4) 0.005(4) 0.005(3) C25 0.023(4) 0.026(4) 0.039(6) 0.000(4) 0.004(4) 0.003(3) C26 0.048(5) 0.040(5) 0.045(6) 0.008(5) 0.003(4) 0.004(4) C27 0.031(4) 0.033(4) 0.038(6) 0.007(4) 0.004(4) 0.001(3) C28 0.040(4) 0.038(5) 0.034(5) 0.009(5) -0.002(4) 0.003(4) C29 0.041(4) 0.028(4) 0.034(5) 0.009(4) 0.001(4) 0.010(3) C30 0.027(4) 0.024(4) 0.040(5) 0.007(4) 0.002(4) 0.001(3) C31 0.030(4) 0.027(4) 0.027(5) 0.001(4) 0.009(3) 0.004(3) C32 0.029(4) 0.023(4) 0.036(5) 0.010(4) 0.004(4) 0.003(3) C33 0.025(4) 0.029(4) 0.040(6) 0.004(5) 0.003(4) 0.008(3) C34 0.043(5) 0.031(4) 0.038(6) 0.012(5) 0.002(4) 0.013(4) C35 0.037(4) 0.026(4) 0.044(6) 0.006(5) -0.004(4) 0.004(3) C36 0.032(4) 0.043(5) 0.036(5) 0.006(5) -0.003(4) 0.008(4) C37 0.030(4) 0.042(5) 0.035(6) 0.013(5) 0.003(4) 0.000(3) C38 0.029(4) 0.029(4) 0.048(6) 0.006(5) 0.004(4) 0.008(3) C39 0.055(5) 0.050(5) 0.043(6) 0.009(5) -0.009(4) 0.004(4) C40 0.087(9) 0.068(8) 0.112(12) 0.018(9) 0.000(9) 0.012(7) C41 0.060(13) 0.053(13) 0.11(2) 0.038(16) -0.033(14) -0.026(11) O7 0.112(13) 0.154(17) 0.079(12) 0.091(13) 0.059(11) 0.069(12) O1S 0.103(12) 0.072(10) 0.072(11) 0.029(9) -0.024(9) 0.001(9) O4A 0.061(11) 0.035(10) 0.045(13) 0.018(8) 0.015(8) 0.009(7) O6A 0.079(12) 0.057(12) 0.062(13) 0.031(9) 0.010(9) 0.003(9) O5A 0.084(14) 0.067(15) 0.073(15) 0.031(10) 0.020(9) -0.014(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.147(7) . ? Ag1 N1 2.158(6) . ? Ag2 N7 2.212(6) 2_665 ? Ag2 N7 2.212(6) . ? Ag2 O2 2.967(5) . ? S1 O5A 1.28(4) . ? S1 O6 1.345(10) . ? S1 O4A 1.45(2) . ? S1 O5 1.448(11) . ? S1 O4 1.479(10) . ? S1 O6A 1.68(3) . ? S1 C40 1.824(13) . ? S2 O9 1.439(11) . ? S2 O8 1.441(13) . ? S2 O7 1.452(14) . ? S2 C41 1.819(19) . ? S2 S2 1.900(10) 2_755 ? S2 O9 1.944(14) 2_755 ? S2 O8 1.955(12) 2_755 ? F1 C40 1.378(16) . ? F2 C40 1.255(14) . ? F3 C40 1.268(14) . ? F4 C41 1.14(3) . ? F5 C41 1.38(2) . ? F6 C41 1.43(3) . ? O1 C6 1.218(10) . ? O2 C19 1.235(9) . ? O3 C32 1.219(8) . ? O8 O9 1.533(17) 2_755 ? O8 S2 1.955(12) 2_755 ? O9 O8 1.533(17) 2_755 ? O9 S2 1.944(14) 2_755 ? N1 C1 1.337(10) . ? N1 C5 1.340(9) . ? N2 C6 1.368(10) . ? N2 C4 1.394(10) . ? N3 C6 1.380(10) . ? N3 C7 1.423(10) . ? N4 C14 1.349(10) . ? N4 C18 1.361(9) . ? N5 C19 1.364(10) . ? N5 C17 1.396(9) . ? N6 C19 1.375(9) . ? N6 C20 1.406(10) . ? N7 C27 1.342(10) . ? N7 C31 1.345(8) . ? N8 C32 1.379(10) . ? N8 C30 1.401(9) . ? N9 C32 1.378(8) . ? N9 C33 1.400(10) . ? C1 C2 1.356(11) . ? C2 C3 1.377(11) . ? C3 C4 1.388(11) . ? C4 C5 1.388(10) . ? C7 C12 1.383(11) . ? C7 C8 1.406(11) . ? C8 C9 1.386(12) . ? C9 C10 1.369(13) . ? C10 C11 1.400(12) . ? C10 C13 1.498(12) . ? C11 C12 1.378(11) . ? C14 C15 1.366(11) . ? C15 C16 1.371(11) . ? C16 C17 1.392(11) . ? C17 C18 1.391(10) . ? C20 C25 1.384(10) . ? C20 C21 1.403(10) . ? C21 C22 1.393(11) . ? C22 C23 1.401(11) . ? C23 C24 1.385(10) . ? C23 C26 1.489(11) . ? C24 C25 1.388(10) . ? C27 C28 1.380(10) . ? C28 C29 1.389(10) . ? C29 C30 1.384(11) . ? C30 C31 1.393(10) . ? C33 C34 1.397(10) . ? C33 C38 1.399(11) . ? C34 C35 1.370(11) . ? C35 C36 1.387(11) . ? C36 C37 1.394(11) . ? C36 C39 1.507(11) . ? C37 C38 1.391(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N1 168.5(2) . . ? N7 Ag2 N7 180.0(3) 2_665 . ? N7 Ag2 O2 85.64(19) 2_665 . ? N7 Ag2 O2 94.36(19) . . ? O5A S1 O6 139.0(18) . . ? O5A S1 O4A 125.0(19) . . ? O6 S1 O4A 69.7(11) . . ? O5A S1 O5 30.8(15) . . ? O6 S1 O5 117.7(7) . . ? O4A S1 O5 151.2(10) . . ? O5A S1 O4 79.6(18) . . ? O6 S1 O4 117.2(8) . . ? O4A S1 O4 49.4(9) . . ? O5 S1 O4 110.4(7) . . ? O5A S1 O6A 110.8(19) . . ? O6 S1 O6A 35.5(9) . . ? O4A S1 O6A 104.4(13) . . ? O5 S1 O6A 83.7(11) . . ? O4 S1 O6A 146.4(10) . . ? O5A S1 C40 109.6(18) . . ? O6 S1 C40 102.3(8) . . ? O4A S1 C40 102.4(10) . . ? O5 S1 C40 102.7(6) . . ? O4 S1 C40 104.0(6) . . ? O6A S1 C40 102.2(11) . . ? O9 S2 O8 113.3(8) . . ? O9 S2 O7 118.5(8) . . ? O8 S2 O7 113.4(10) . . ? O9 S2 C41 102.9(9) . . ? O8 S2 C41 107.0(11) . . ? O7 S2 C41 99.4(13) . . ? O9 S2 S2 69.6(6) . 2_755 ? O8 S2 S2 70.1(5) . 2_755 ? O7 S2 S2 91.4(9) . 2_755 ? C41 S2 S2 169.0(10) . 2_755 ? O9 S2 O9 113.6(6) . 2_755 ? O8 S2 O9 51.3(6) . 2_755 ? O7 S2 O9 70.8(10) . 2_755 ? C41 S2 O9 142.5(8) . 2_755 ? S2 S2 O9 44.0(4) 2_755 2_755 ? O9 S2 O8 51.0(6) . 2_755 ? O8 S2 O8 114.0(5) . 2_755 ? O7 S2 O8 74.5(8) . 2_755 ? C41 S2 O8 137.6(10) . 2_755 ? S2 S2 O8 43.9(4) 2_755 2_755 ? O9 S2 O8 76.2(5) 2_755 2_755 ? C19 O2 Ag2 122.2(5) . . ? S2 O8 O9 81.6(9) . 2_755 ? S2 O8 S2 66.0(5) . 2_755 ? O9 O8 S2 46.8(5) 2_755 2_755 ? S2 O9 O8 82.2(8) . 2_755 ? S2 O9 S2 66.4(6) . 2_755 ? O8 O9 S2 47.2(6) 2_755 2_755 ? C1 N1 C5 119.4(7) . . ? C1 N1 Ag1 117.0(5) . . ? C5 N1 Ag1 123.4(6) . . ? C6 N2 C4 128.3(7) . . ? C6 N3 C7 127.4(7) . . ? C14 N4 C18 119.1(7) . . ? C14 N4 Ag1 122.6(5) . . ? C18 N4 Ag1 118.2(5) . . ? C19 N5 C17 128.8(7) . . ? C19 N6 C20 125.4(7) . . ? C27 N7 C31 119.5(6) . . ? C27 N7 Ag2 118.0(5) . . ? C31 N7 Ag2 121.9(5) . . ? C32 N8 C30 127.6(6) . . ? C32 N9 C33 125.1(6) . . ? N1 C1 C2 121.5(8) . . ? C1 C2 C3 120.2(8) . . ? C2 C3 C4 119.1(8) . . ? C5 C4 C3 117.7(7) . . ? C5 C4 N2 125.4(8) . . ? C3 C4 N2 116.8(7) . . ? N1 C5 C4 122.1(8) . . ? O1 C6 N2 124.8(7) . . ? O1 C6 N3 124.9(8) . . ? N2 C6 N3 110.3(8) . . ? C12 C7 C8 118.6(7) . . ? C12 C7 N3 124.4(7) . . ? C8 C7 N3 116.9(8) . . ? C9 C8 C7 119.8(9) . . ? C10 C9 C8 122.5(8) . . ? C9 C10 C11 116.6(8) . . ? C9 C10 C13 121.0(9) . . ? C11 C10 C13 122.4(10) . . ? C12 C11 C10 122.7(9) . . ? C11 C12 C7 119.8(8) . . ? N4 C14 C15 121.1(8) . . ? C14 C15 C16 120.7(8) . . ? C15 C16 C17 119.3(8) . . ? C18 C17 C16 118.1(7) . . ? C18 C17 N5 124.4(7) . . ? C16 C17 N5 117.5(7) . . ? N4 C18 C17 121.7(7) . . ? O2 C19 N5 122.9(7) . . ? O2 C19 N6 124.3(7) . . ? N5 C19 N6 112.8(7) . . ? C25 C20 C21 119.2(7) . . ? C25 C20 N6 121.9(6) . . ? C21 C20 N6 118.9(7) . . ? C22 C21 C20 119.6(8) . . ? C21 C22 C23 121.6(7) . . ? C24 C23 C22 117.2(7) . . ? C24 C23 C26 122.1(7) . . ? C22 C23 C26 120.7(7) . . ? C23 C24 C25 122.2(7) . . ? C20 C25 C24 120.2(7) . . ? N7 C27 C28 121.8(7) . . ? C27 C28 C29 118.9(7) . . ? C30 C29 C28 119.6(7) . . ? C29 C30 C31 118.3(7) . . ? C29 C30 N8 116.9(6) . . ? C31 C30 N8 124.7(7) . . ? N7 C31 C30 121.8(7) . . ? O3 C32 N9 124.0(7) . . ? O3 C32 N8 123.6(7) . . ? N9 C32 N8 112.4(6) . . ? C34 C33 C38 118.0(7) . . ? C34 C33 N9 118.8(7) . . ? C38 C33 N9 123.2(7) . . ? C35 C34 C33 121.3(8) . . ? C34 C35 C36 121.1(7) . . ? C35 C36 C37 118.2(7) . . ? C35 C36 C39 121.4(7) . . ? C37 C36 C39 120.3(8) . . ? C38 C37 C36 121.0(8) . . ? C37 C38 C33 120.3(7) . . ? F2 C40 F3 113.3(14) . . ? F2 C40 F1 103.8(11) . . ? F3 C40 F1 103.5(14) . . ? F2 C40 S1 114.2(10) . . ? F3 C40 S1 112.0(9) . . ? F1 C40 S1 109.0(10) . . ? F4 C41 F5 111(2) . . ? F4 C41 F6 117.0(18) . . ? F5 C41 F6 100(2) . . ? F4 C41 S2 113(2) . . ? F5 C41 S2 107.7(13) . . ? F6 C41 S2 106.5(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O5A 0.88 1.91 2.72(4) 152.0 1_665 N2 H2 O5 0.88 2.15 2.929(13) 147.8 1_665 N3 H3 O4 0.88 2.19 3.043(16) 164.7 1_665 N3 H3 O5A 0.88 2.20 2.97(4) 145.8 1_665 N5 H5 O4A 0.88 2.10 2.96(3) 163.4 . N5 H5 O6 0.88 2.10 2.905(15) 151.5 . N6 H6 O6 0.88 1.98 2.783(12) 150.8 . N6 H6 O6A 0.88 2.13 2.95(3) 154.5 . N8 H8 O7 0.88 2.22 3.033(17) 153.9 . N8 H8 O9 0.88 2.36 3.153(13) 150.7 2_755 N9 H9 O7 0.88 2.04 2.881(16) 159.3 . N9 H9 O1S 0.88 2.17 2.920(16) 142.5 . _diffrn_measured_fraction_theta_max 0.594 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.594 _refine_diff_density_max 0.723 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.102 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Jonathan Steed' _publ_contact_author_address ; Department of Chemistry University of Durham South Road Durham DH1 3QY UNITED KINGDOM ; _publ_contact_author_email JON.STEED@DURHAM.AC.UK _publ_section_title ; A Modular, Self-Assembled, Separated Ion-Pair Binding System ; loop_ _publ_author_name 'Jonathan Steed' 'Judith A. K. Howard' 'Elinor C. Spencer' 'Derek A. Tocher' 'David R. Turner' data_str0192 _database_code_depnum_CCDC_archive 238925 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H52 Ag2 N12 O8 S' _chemical_formula_weight 1220.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 17.4146(6) _cell_length_b 17.4146(6) _cell_length_c 8.2655(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2506.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.892 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7634 _exptl_absorpt_correction_T_max 0.9321 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21760 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3055 _reflns_number_gt 2908 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.9264P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 3055 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.0000 0.5000 0.18502(3) 0.04582(10) Uani 1 2 d S . . O1 O 0.81794(9) 0.52835(11) 0.6562(2) 0.0334(4) Uani 1 1 d . . . N1 N 0.88337(10) 0.47125(13) 0.1971(3) 0.0318(4) Uani 1 1 d . . . N2 N 0.72157(9) 0.49781(13) 0.4782(2) 0.0247(3) Uani 1 1 d . . . H2B H 0.6714 0.4961 0.4661 0.030 Uiso 1 1 calc R . . N3 N 0.69118(10) 0.54412(11) 0.7265(2) 0.0242(4) Uani 1 1 d . . . H3B H 0.6442 0.5385 0.6889 0.029 Uiso 1 1 calc R . . C1 C 0.85025(15) 0.42663(18) 0.0860(3) 0.0401(6) Uani 1 1 d . . . H1A H 0.8796 0.4096 -0.0039 0.048 Uiso 1 1 calc R . . C2 C 0.77376(16) 0.40450(17) 0.0986(4) 0.0403(6) Uani 1 1 d . . . H2A H 0.7506 0.3737 0.0173 0.048 Uiso 1 1 calc R . . C3 C 0.73224(13) 0.42806(15) 0.2310(3) 0.0309(5) Uani 1 1 d . . . H3A H 0.6802 0.4128 0.2425 0.037 Uiso 1 1 calc R . . C4 C 0.76602(12) 0.47392(13) 0.3475(3) 0.0228(4) Uani 1 1 d . . . C5 C 0.84240(11) 0.49548(15) 0.3251(3) 0.0265(4) Uani 1 1 d . . . H5A H 0.8661 0.5282 0.4024 0.032 Uiso 1 1 calc R . . C6 C 0.74901(12) 0.52397(13) 0.6249(3) 0.0240(4) Uani 1 1 d . . . C7 C 0.69766(12) 0.57318(12) 0.8863(3) 0.0231(4) Uani 1 1 d . . . C8 C 0.76460(13) 0.60378(14) 0.9522(3) 0.0275(5) Uani 1 1 d . . . H8A H 0.8114 0.6020 0.8932 0.033 Uiso 1 1 calc R . . C9 C 0.76241(14) 0.63684(14) 1.1047(3) 0.0300(5) Uani 1 1 d . . . H9A H 0.8080 0.6587 1.1479 0.036 Uiso 1 1 calc R . . C10 C 0.69525(13) 0.63898(13) 1.1969(3) 0.0267(5) Uani 1 1 d . . . C11 C 0.63037(13) 0.60448(13) 1.1321(3) 0.0273(5) Uani 1 1 d . . . H11A H 0.5845 0.6029 1.1941 0.033 Uiso 1 1 calc R . . C12 C 0.63108(12) 0.57236(13) 0.9792(3) 0.0251(5) Uani 1 1 d . . . H12A H 0.5857 0.5495 0.9372 0.030 Uiso 1 1 calc R . . C13 C 0.69192(17) 0.67908(17) 1.3592(3) 0.0393(6) Uani 1 1 d . . . H13A H 0.6401 0.6744 1.4042 0.059 Uiso 1 1 calc R . . H13B H 0.7046 0.7335 1.3452 0.059 Uiso 1 1 calc R . . H13C H 0.7289 0.6553 1.4332 0.059 Uiso 1 1 calc R . . S1 S 0.0000 0.0000 0.0000 0.01705(17) Uani 1 4 d S . . O2 O 0.05745(9) 0.03994(9) 0.1012(2) 0.0284(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01336(11) 0.0889(2) 0.03525(14) 0.000 0.000 -0.00046(15) O1 0.0175(7) 0.0479(10) 0.0348(9) -0.0028(7) -0.0034(6) 0.0020(7) N1 0.0158(8) 0.0450(11) 0.0345(10) 0.0024(9) -0.0010(8) 0.0045(8) N2 0.0140(7) 0.0296(8) 0.0305(8) -0.0018(10) 0.0000(6) -0.0019(8) N3 0.0174(8) 0.0280(10) 0.0273(9) 0.0011(7) -0.0012(7) -0.0022(7) C1 0.0251(12) 0.0569(17) 0.0382(14) -0.0117(13) 0.0044(10) 0.0096(11) C2 0.0281(13) 0.0502(17) 0.0427(16) -0.0186(13) -0.0018(11) -0.0002(11) C3 0.0201(10) 0.0334(12) 0.0391(13) -0.0060(11) 0.0013(9) -0.0044(9) C4 0.0171(9) 0.0222(9) 0.0290(11) 0.0042(8) -0.0009(8) 0.0023(7) C5 0.0171(8) 0.0308(10) 0.0318(10) 0.0034(12) -0.0031(7) 0.0001(9) C6 0.0198(10) 0.0234(10) 0.0289(10) 0.0064(9) -0.0024(8) 0.0011(7) C7 0.0212(10) 0.0212(10) 0.0269(10) 0.0066(9) -0.0025(8) 0.0008(8) C8 0.0222(10) 0.0326(12) 0.0277(11) 0.0086(9) 0.0001(9) -0.0060(9) C9 0.0271(11) 0.0334(13) 0.0295(12) 0.0096(10) -0.0085(10) -0.0091(10) C10 0.0282(11) 0.0245(11) 0.0274(11) 0.0035(9) -0.0037(9) 0.0005(9) C11 0.0236(11) 0.0268(11) 0.0314(12) 0.0017(9) -0.0002(9) 0.0042(8) C12 0.0197(10) 0.0233(10) 0.0323(12) 0.0022(9) -0.0043(9) 0.0023(8) C13 0.0412(14) 0.0429(15) 0.0337(14) -0.0060(11) -0.0040(11) 0.0000(12) S1 0.0142(2) 0.0142(2) 0.0227(4) 0.000 0.000 0.000 O2 0.0246(8) 0.0225(8) 0.0379(9) -0.0068(7) -0.0093(7) 0.0007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic= ) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.0941(19) 2_765 ? Ag1 N1 2.0941(19) . ? O1 C6 1.230(3) . ? N1 C1 1.334(4) . ? N1 C5 1.344(3) . ? N2 C6 1.381(3) . ? N2 C4 1.393(3) . ? N3 C6 1.357(3) . ? N3 C7 1.419(3) . ? C1 C2 1.391(4) . ? C2 C3 1.374(4) . ? C3 C4 1.382(3) . ? C4 C5 1.394(3) . ? C7 C12 1.390(3) . ? C7 C8 1.393(3) . ? C8 C9 1.386(4) . ? C9 C10 1.396(3) . ? C10 C11 1.387(3) . ? C10 C13 1.514(4) . ? C11 C12 1.382(3) . ? S1 O2 1.4778(15) . ? S1 O2 1.4778(15) 2 ? S1 O2 1.4778(15) 3 ? S1 O2 1.4778(15) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 174.55(12) 2_765 . ? C1 N1 C5 119.7(2) . . ? C1 N1 Ag1 121.73(17) . . ? C5 N1 Ag1 118.50(16) . . ? C6 N2 C4 125.99(17) . . ? C6 N3 C7 127.53(19) . . ? N1 C1 C2 121.6(2) . . ? C3 C2 C1 118.8(2) . . ? C2 C3 C4 120.2(2) . . ? C3 C4 N2 118.4(2) . . ? C3 C4 C5 118.0(2) . . ? N2 C4 C5 123.5(2) . . ? N1 C5 C4 121.7(2) . . ? O1 C6 N3 125.3(2) . . ? O1 C6 N2 122.8(2) . . ? N3 C6 N2 111.84(18) . . ? C12 C7 C8 119.1(2) . . ? C12 C7 N3 116.3(2) . . ? C8 C7 N3 124.5(2) . . ? C9 C8 C7 119.4(2) . . ? C8 C9 C10 122.0(2) . . ? C11 C10 C9 117.4(2) . . ? C11 C10 C13 120.7(2) . . ? C9 C10 C13 121.9(2) . . ? C12 C11 C10 121.4(2) . . ? C11 C12 C7 120.5(2) . . ? O2 S1 O2 111.08(14) . 2 ? O2 S1 O2 108.67(7) . 3 ? O2 S1 O2 108.67(7) 2 3 ? O2 S1 O2 108.67(7) . 4 ? O2 S1 O2 108.67(7) 2 4 ? O2 S1 O2 111.08(14) 3 4 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 N1 C1 -147.1(2) 2_765 . . . ? N1 Ag1 N1 C5 29.42(18) 2_765 . . . ? C5 N1 C1 C2 0.3(4) . . . . ? Ag1 N1 C1 C2 176.7(2) . . . . ? N1 C1 C2 C3 -1.5(5) . . . . ? C1 C2 C3 C4 1.0(4) . . . . ? C2 C3 C4 N2 178.8(2) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C6 N2 C4 C3 160.3(2) . . . . ? C6 N2 C4 C5 -21.6(4) . . . . ? C1 N1 C5 C4 1.4(4) . . . . ? Ag1 N1 C5 C4 -175.23(17) . . . . ? C3 C4 C5 N1 -1.7(3) . . . . ? N2 C4 C5 N1 -179.9(2) . . . . ? C7 N3 C6 O1 -0.5(4) . . . . ? C7 N3 C6 N2 180.0(2) . . . . ? C4 N2 C6 O1 -0.6(4) . . . . ? C4 N2 C6 N3 179.0(2) . . . . ? C6 N3 C7 C12 -165.2(2) . . . . ? C6 N3 C7 C8 16.8(3) . . . . ? C12 C7 C8 C9 -3.8(3) . . . . ? N3 C7 C8 C9 174.2(2) . . . . ? C7 C8 C9 C10 1.5(3) . . . . ? C8 C9 C10 C11 1.9(3) . . . . ? C8 C9 C10 C13 -176.5(2) . . . . ? C9 C10 C11 C12 -2.9(3) . . . . ? C13 C10 C11 C12 175.4(2) . . . . ? C10 C11 C12 C7 0.6(3) . . . . ? C8 C7 C12 C11 2.8(3) . . . . ? N3 C7 C12 C11 -175.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.500 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.058